Tamsulosin Hydrochloride Capsules

This article is compiled based on the United States Pharmacopeia (USP) – 2025 Edition

Issued and maintained by the United States Pharmacopeial Convention (USP)

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1 DEFINITION

Tamsulosin Hydrochloride Capsules contain NLT 90.0% and NMT 110.0% of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl).

2 IDENTIFICATION

A. The retention time of the tamsulosin peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

B. The UV spectrum of the tamsulosin peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay.

3 ASSAY

Change to read:

Procedure 1

Solution A: Dilute 20 mL of hydrochloric acid with water to 1000 mL.

Solution B: Dissolve 8.7 mL of perchloric acid and 3.0 g of sodium hydroxide in 1900 mL of water. Adjust with 1 N sodium hydroxide to a pH of 2.0, and dilute with water to 2000 mL.

Mobile phase: Acetonitrile and Solution B (30:70)

Diluent: Water and acetonitrile (70:30)

Internal standard solution: 0.4 mg/mL of Propylparaben in Diluent

Standard stock solution: 0.5 mg/mL of USP Tamsulosin Hydrochloride RS in Diluent

Standard solution: 0.025 mg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution and 0.05 mg/mL of propylparaben from the Internal standard solution in Mobile phase

Sample solution: Nominally 0.025 mg/mL of tamsulosin hydrochloride from Capsules and 0.05 mg/mL of propylparaben from the Internal standard solution prepared as follows. Transfer an amount equivalent to about 1 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a Te on-lined, screw-capped centrifuge tube. Place approximately 100 glass balls with a diameter of about 5 mm into the tube, add 20 mL of 0.05 N sodium hydroxide, heat at 50° for 10 min, and shake well for 30 min.

Add 15 mL of a mixture of acetonitrile and Solution A (2:1), and shake well. Add 5.0 mL of the Internal standard solution, and shake well.

Centrifuge at 1500 rpm for 10 min, and use the supernatant, passing it, if necessary, through a membrane fIlter of 0.5-μm or smaller pore size.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm. For Identification B, use a diode array detector in the range of 200–400 nm.

Column: 4.0-mm × 15-cm or 4.6-mm × 15-cm; 5-μm packing L1

Column temperature: 40°

Flow rate: 1.0 mL/min for the 4.0-mm column and 1.3 mL/min for the 4.6-mm column. [Note—The flow rate can be adjusted as needed to achieve a recommended retention time of approximately 6 min for tamsulosin.]

Injection volume: 10 μL

System suitability

Sample: Standard solution

Suitability requirements

Resolution: NLT 12 between tamsulosin and propylparaben. [Note—The elution order is tamsulosin hydrochloride followed by propylparaben.]

Relative standard deviation: NMT 2.0% for the ratios of the peak areas for tamsulosin and the internal standard

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the portion of Capsules taken:

Result = (R_U/R_S) × (C_S/C_U) × 100

R_U = peak area ratio of tamsulosin to the internal standard from the Sample solution

R_S = peak area ratio of tamsulosin to the internal standard from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard (ERR 1-Dec-2024) solution (mg/mL)

C_U = nominal concentration of tamsulosin hydrochloride in the Sample solution (mg/mL)

Acceptance criteria: 90.0%–110.0%

Procedure 2: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 2.

Solution B and Mobile phase: Prepare as directed for Procedure 1.

Buffer: Dissolve 3.4 g of monobasic potassium phosphate in 1 L of water. Adjust with 2 N sodium hydroxide to a pH of 5.80 ± 0.05.

Standard solution: 0.0032 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Dissolve 1.2 mg/mL of USP Tamsulosin

Hydrochloride RS in methanol. Further dilute this solution with Buffer to 3.2 μg/mL.

Sample solution: Nominally 0.0032 mg/mL of tamsulosin hydrochloride prepared as follows. Transfer an amount equivalent to 1.6 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a 100-mL volumetric flask. Add 20 mL of methanol, stir for 30 min, sonicate for 30 min, and stir again for 30 min. Add 40 mL of methanol, sonicate for another 30 min, and stir for another 60 min. Dilute with methanol to volume, mix well, and allow the solution to stand for 5 min. Dilute 5 mL of this solution with

Buffer to 25 mL, and allow the solution to stand for 5 min. Pass through a PVDF fIlter of 0.45-μm pore size, discarding the first 5 mL of the filtrate.

Chromatographic system: Proceed as directed for Procedure 1, except for Injection volume.

Injection volume: 50 μL

System suitability

Sample: Standard solution

Suitability requirements

Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the portion of Capsules taken:

Result = (r_U/r _S) × (C_S /C_U ) × 100

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS from the Standard solution (mg/mL)

C_U = nominal concentration of tamsulosin hydrochloride from the Sample solution (mg/mL)

Acceptance criteria: 90.0%–110.0%

Procedure 3: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 3.

Solution B and Mobile phase: Prepare as directed for Procedure 1.

Buffer: 6.9 g/L of monobasic sodium phosphate monohydrate in water. Adjust with 5 N sodium hydroxide to a pH of 7.2 ± 0.05.

Standard solution: 0.03 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Dissolve 0.5 mg/mL of USP Tamsulosin

Hydrochloride RS in a mixture of methanol and water (50:50). Further dilute a portion of this solution with methanol to 0.03 mg/mL.

Sample solution: Nominally 0.03 mg/mL of tamsulosin hydrochloride from Capsules prepared as follows. Transfer an amount equivalent to 0.8 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a 25-mL volumetric flask. Add 5 mL of Buffer, shake for 15 min, add 10 mL of methanol, shake for 1 h, and dilute with methanol to volume. Pass through a suitable fIlter of 0.45-μm pore size.

Chromatographic system: Proceed as directed for Procedure 1, except for Injection volume.

Injection volume: 20 μL

System suitability and Analysis: Proceed as directed for Procedure 2.

Acceptance criteria: 90.0%–110.0%

Procedure 4: For Capsules labeled to meet the requirements of Dissolution Test 4, proceed as directed for Procedure 1.

Procedure 5: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 5.

Solution B, Mobile phase, and Chromatographic system: Proceed as directed for Procedure 1.

Diluent: Methanol and water (75:25)

Standard solution: 0.016 mg/mL of USP Tamsulosin Hydrochloride RS in Diluent

Sample solution: Nominally 0.016 mg/mL of tamsulosin hydrochloride from Capsules prepared as follows. Transfer the contents of 10

Capsules (equivalent to 4 mg of tamsulosin hydrochloride) into a 250-mL volumetric flask. Add 200 mL of Diluent, stir, and sonicate simultaneously for at least 2 h. Cool, and dilute with Diluent to volume. Pass through a suitable fIlter.

System suitability and Analysis: Proceed as directed for Procedure 2.

Acceptance criteria: 90.0%–110.0%

Procedure 6: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 6.

Solution B and Mobile phase: Prepare as directed for Procedure 1.

Buffer: Dissolve 6.8 g/L of monobasic potassium phosphate and 0.9 g/L of sodium hydroxide in water. Adjust with sodium hydroxide solution to a pH of 6.8.

Diluent 1: Acetonitrile and Buffer (50:50)

Diluent 2: Acetonitrile and Solution B (50:50)

Standard solution: 0.008 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Dissolve 0.4 mg/mL of USP Tamsulosin

Hydrochloride RS in Diluent 1, using sonication as necessary. Further dilute the solution with Diluent 2 to 0.008 mg/mL.

Sample solution: Nominally 0.008 mg/mL of tamsulosin hydrochloride from Capsules prepared as follows. Transfer an amount equivalent to 4 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a 100-mL volumetric flask. Add 60 mL of Diluent 1, and sonicate with intermittent shaking to disperse the pellets completely. Cool, and dilute with Diluent 1 to volume. Centrifuge, transfer 5 mL of supernatant solution to a 25-mL volumetric flask, and dilute with Diluent 2 to volume. Pass through a nylon membrane fIlter of 0.45-μm pore size.

Chromatographic system: Proceed as directed for Procedure 1, except for Injection volume.

Injection volume: 20 μL

System suitability and Analysis: Proceed as directed for Procedure 2.

Acceptance criteria: 90.0%–110.0%

Procedure 7: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 7.

Solution B and Mobile phase: Prepare as directed for Procedure 1.

Buffer: Dissolve 76 g/L of tribasic sodium phosphate in water.

Diluent: 0.1 N hydrochloric acid and Buffer (75:25), adjusted with diluted hydrochloric acid or sodium hydroxide solution to a pH of 7.0

Standard solution: 0.0016 mg/mL of USP Tamsulosin Hydrochloride RS in Diluent

Sample solution: Nominally 0.0016 mg/mL of tamsulosin hydrochloride from Capsules prepared as follows. Transfer an amount equivalent to 0.4 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a 250-mL volumetric flask, and dilute with Diluent to volume. Stir for 24 h by mechanical means at 40° protected from light. Pass through a suitable fIlter of 0.45-μm pore size.

Chromatographic system: Proceed as directed for Procedure 1, except for Injection volume.

Injection volume: 50 μL

System suitability and Analysis: Proceed as directed for Procedure 2.

Acceptance criteria: 90.0%–110.0%

Procedure 8: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 8.

Solution B, Mobile phase, and Chromatographic system: Proceed as directed for Procedure 1.

Standard solution: 0.025 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Dissolve 0.1 mg/mL of USP Tamsulosin

Hydrochloride RS in methanol. Further dilute the solution to 0.025 mg/mL of USP Tamsulosin Hydrochloride RS in Mobile phase.

Sample solution: Nominally 0.025 mg/mL of tamsulosin hydrochloride from Capsules prepared as follows. Transfer an amount equivalent to 2.5 mg of tamsulosin hydrochloride, from a portion of the weighed and mixed contents of the Capsules (NLT 20), into a 100-mL volumetric flask. Add 25 mL of 0.1 N sodium hydroxide, and sonicate for 30 min. Add 30 mL of Mobile phase, shake by mechanical means for 30 min, and dilute with Mobile phase to volume. Centrifuge, and pass through a PVDF membrane fIlter of 0.45-μm pore size, discarding the first few milliliters of the filtrate.

System suitability and Analysis: Proceed as directed for Procedure 2.

Acceptance criteria: 90.0%–110.0%

Procedure 9: For Capsules labeled to meet the requirements of Dissolution Test 9, proceed as directed for Procedure 1.

Procedure 10: Use this procedure for Capsules labeled to meet the requirements of Dissolution Test 10.

Solution A, Solution B, Mobile phase, and Diluent: Prepare as directed for Procedure 1.

Internal standard solution: 0.5 mg/mL of propylparaben in Diluent

Standard stock solution: 0.62 mg/mL of USP Tamsulosin Hydrochloride RS in Diluent

Standard solution: 0.025 mg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution and 0.05 mg/mL of propylparaben from the Internal standard solution in Mobile phase.

Sample solution: Nominally 0.025 mg/mL of tamsulosin hydrochloride from Capsules and 0.05 mg/mL of propylparaben from the Internal standard solution prepared as follows. Transfer an amount equivalent to 1.2 mg of tamsulosin hydrochloride, from a portion of the weighed, mixed, and crushed contents of the Capsules (NLT 20), into a 50-mL volumetric flask. Add 25 mL of 0.05 N sodium hydroxide solution, heat at 50° for 15 min, and shake mechanically for 60 min. Sonicate for 30 min with intermittent shaking and add 15 mL of a mixture of Solution

A and acetonitrile (1:2). Sonicate for another 15 min with intermittent shaking. Add 5 mL of Internal standard solution, dilute with a mixture of Solution A and acetonitrile (1:2) to volume, and mix well. Centrifuge the solution for 10 min and pass the solution through a suitable glass fiber fIlter.

Chromatographic system: Proceed as directed for Procedure 1.

System suitability

Sample: Standard solution

Suitability requirements

Resolution: NLT 12 between tamsulosin and propylparaben. [Note—The elution order is tamsulosin hydrochloride followed by propylparaben.]

Relative standard deviation: NMT 2.0% for each peak

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the portion of Capsules taken:

Result = (R_U/R_S) × (C_S/C_U ) × 100

R_U = peak area ratio of tamsulosin to the internal standard from the Sample solution

R_S = peak area ratio of tamsulosin to the internal standard from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (mg/mL)

C_U = nominal concentration of tamsulosin hydrochloride in the Sample solution (mg/mL)

Acceptance criteria: 90.0%–110.0%

4 PERFORMANCE TESTS

Change to read:

Dissolution 〈711〉

Test 1

Solution B, Mobile phase, Diluent, and Standard stock solution: Prepare as directed in the Assay, Procedure 1.

Acid stage medium: Dissolve 2.0 g of sodium chloride in 5.7 mL of hydrochloric acid, and dilute to 1000 mL with water. To 500 mL of this fluid, add 1 mL of Polysorbate 80 aqueous solution (3 g in 200 mL of water) just before the test; 500 mL.

Buffer stage medium: pH 7.2 phosphate buffer. Dissolve 6.8 g of monobasic potassium phosphate in 250 mL of water, add 90 mL of 0.2 N sodium hydroxide and 500 mL of water, adjust with 0.2 N sodium hydroxide or 0.2 N hydrochloric acid to a pH of 7.2 ± 0.05, and dilute with water to 1000 mL; 500 mL

Apparatus 2: 100 rpm, with sinker (see Dissolution 〈711〉, Figure 2a)

Times: 2, 3, and 8 h

Internal standard solution: 0.008 mg/mL of propylparaben in Diluent

Standard solution: 0.67 μg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution and 1.3 μg/mL of propylparaben from

the Internal standard solution in Acid stage medium prepared as follows. Transfer 4.0 mL of the Standard stock solution to a 100-mL volumetric flask, and dilute to volume with Acid stage medium. Transfer 4.0 mL of this dilution to another 100-mL volumetric flask, and dilute with Acid stage medium to volume. Transfer 10.0 mL of this last dilution to a test tube, and add 2.0 mL of the Internal standard solution.

Procedure: After 2 h in Acid stage medium, withdraw 10.0 mL of solution under test and immediately drain the Acid stage medium by suction through a tube capped with a 60-mesh stainless wire screen. Rinse the drain tube while adding Buffer stage medium previously warmed, and continue test. After 3 h (including the 2 h in the Acid stage medium), withdraw 10.0 mL of the solution under test and replace with the same volume of Buffer stage medium. After 8 h (including the 2 h in the Acid stage medium), withdraw 10.0 mL of the solution under test.

Sample solutions

Acid stage sample: Add 2.0 mL of the Internal standard solution, mix well, and pass through a suitable fIlter of 0.5-μm pore size, discarding the first 5 mL.

Buffer stage sample: Add 1.0 mL of 0.5 N hydrochloric acid and 2.0 mL of the Internal standard solution, mix well, and pass through a suitable fIlter of 0.5-μm pore size, discarding the first 5 mL.

Chromatographic system: Proceed as directed in the Assay, Procedure 1 except for Injection volume.

Injection volume: 250 μL

Analysis

Samples: Standard solution and Sample solution (either Acid stage sample or Buffer stage sample depending on time point)

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn at each time point (i):

Result_i = (R_U /R_S ) × C_S

R_U = peak area ratio of tamsulosin to the Internal standard from the Sample solution

R_S = peak area ratio of tamsulosin to the Internal standard from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (μg/mL)

Calculate the percentage of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result

Result₃ = {[(C₃ × V₂ ) + (C₂ × (ERR 1-Dec-2024) V_S )] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specied time point (mg/mL)

V₁ = volume of Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of Buffer stage medium, 500 mL

V_S = volume of Sample solution withdrawn at each time point from the medium (mL)

Tolerances: See Table 1.

Table 1

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to Dissolution 〈711〉, Acceptance Table 2.

Test 2: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 2.

Acid stage medium: 0.003% Polysorbate 80, pH 1.2 prepared as follows. For each liter prepared, transfer 8.5 mL of hydrochloric acid to a suitable volumetric flask and add 900 mL of water and 0.03 mL of polysorbate 80. Adjust with 0.2 N sodium hydroxide or 0.2 N hydrochloric acid to a pH of 1.2 ± 0.05, and dilute with water to 1000 mL; 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 100 rpm, with sinkers1

Times: 2 h in the Acid stage medium and 8 h in the Buffer stage medium (including the 2 h in the Acid stage medium)

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium and replace it with the Buffer stage medium previously warmed, and continue the test. At 6 h after the replacement of the Medium, withdraw a sample of the solution under test.

Standard stock solution: 0.5 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Transfer about 25.0 mg of USP Tamsulosin Hydrochloride RS to a 50-mL volumetric flask. Add 25 mL of methanol. Dilute with Buffer stage medium to volume. Sonicate until dissolved.

Standard solution: 0.8 μg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution in Buffer stage medium

Sample solution: Pass a portion of the solution under test through a suitable fIlter.

Buffer: 3.4 g/L of monobasic potassium phosphate in water. Adjust with 2 N sodium hydroxide to a pH of 5.80 ± 0.05.

Mobile phase: Buffer and acetonitrile (3:1)

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 4.6-mm × 15-cm; 5-μm packing L1

Flow rate: 1 mL/min

Injection volume: 50 μL

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the concentration (C_i) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

Tolerances: See Table 2.

Table 2

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to Dissolution 〈711〉, Acceptance Table 2.

Test 3: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 3.

Acid stage medium: 0.003% Polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL Buffer stage concentrate: 0.1 M phosphate buffer, pH 11.6 (138 g of sodium phosphate monohydrate and 320 mL of 5 N sodium hydroxide in 10 L of water. Adjust with 5 N sodium hydroxide to a pH of 11.6 ± 0.05.)

Buffer stage medium: Add 500 mL of the Buffer stage concentrate to the remaining Acid stage medium in each vessel. The final pH is about 7.2, 1000 mL.

Apparatus 2: 100 rpm, with sinkers

Times: 2 h for Acid stage medium and 3 and 8 h for Buffer stage medium (including the 2 h in the Acid stage medium)

Procedure: Perform the test using the Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test and leave the remaining Acid stage medium in the vessel. Add 500 mL of Buffer stage concentrate, and continue test. At 1 and 6 h after the addition of Buffer stage medium, withdraw a sample of the solution under test.

Sample solution: Pass a portion of the solution under test through a suitable fIlter.

Standard stock solution: 0.5 mg/mL of USP Tamsulosin Hydrochloride RS in water and methanol (1:1)

Standard solution: 0.3 μg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution in Buffer stage medium

Sample solution: Pass a portion of the solution under test through a suitable fIlter.

Buffer: 6.8 g/L of monobasic potassium phosphate in water. Adjust with 2 N sodium hydroxide to a pH of 5.5 ± 0.05.

Mobile phase: Buffer and acetonitrile (3:2)

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 275 nm

Column: 4.6-mm × 15-cm; 5-μm packing L1

Column temperature: 30°

Flow rate: 1 mL/min

Injection volume: 100 μL

System suitability

Sample: Standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.5%

Analysis

Samples: Standard solution and Sample solution

Calculate the concentration (C_i) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result_i = (r_U/r_S) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (μg/mL)

Calculate the percentage of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (Q_i)):

Result₁ = C × V₁ × (1/L) × 100

Result₂ = [(C₂ × V₂ ) + (C₁ × V_S )] × (1/L) × 100

Result₃ = {(C₃ × V₂ ) + [(C₂ + C₁ ) × V_S ]} × (1/L) × 100

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specied time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 1000 mL

V_S = volume of the Sample solution withdrawn at each time point from the medium

Tolerances: See Table 3.

Table 3

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 4: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 4.

Acid stage medium: 0.003% Polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 100 rpm

Times: 2 h for the Acid stage medium, and 3 and 8 h for the Buffer stage medium (including the 2 h in the Acid stage medium)

Procedure: Perform the test using the Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 1 and 6 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed. 50 mM sodium perchlorate solution: Dissolve 7.0 g of monohydrate sodium perchlorate in 1 L of water, and add 5 mL of phosphoric acid.

Mobile phase: 50 mM sodium perchlorate solution and acetonitrile (3:2)

Acid stage standard stock solution: Transfer 20 mg of USP Tamsulosin Hydrochloride RS to a 500-mL volumetric flask, add 25 mL of methanol, and sonicate until dissolved. Dilute with Acid stage medium to volume.

Acid stage standard solution: Dilute the Acid stage standard stock solution with Acid stage medium to obtain a final concentration of about 0.08 μg/mL.

Buffer stage standard stock solution: Transfer 20 mg of USP Tamsulosin Hydrochloride RS to a 250-mL volumetric flask, add 25 mL of methanol, and sonicate until dissolved. Dilute with Buffer stage medium to volume.

Buffer stage standard solution: Dilute the Buffer stage standard stock solution with Buffer stage medium to obtain a final concentration of about 0.8 μg/mL.

Sample solution: Pass a portion of the solution under test through a suitable fIlter.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 230 nm

Columns

Guard: 3-mm × 4-cm; packing L1

Analytical: 3.9-mm × 15-cm; 5-μm packing L1

Column temperature: 35°

Flow rate: 1.5 mL/min

Injection volume: 200 μL

System suitability

Samples: Acid stage standard solution and Buffer stage standard solution

Suitability requirements

Relative standard deviation: NMT 3.0%, Acid stage standard solution; NMT 1.5%, Buffer stage standard solution

Analysis

Samples: Acid stage standard solution, Buffer stage sample solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the appropriate Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the appropriate Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium (mL)

Tolerances: See Table 4.

Table 4

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified in the Buffer stage conform to Dissolution 〈711〉, Acceptance Table 2.

Test 5: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 5.

Acid stage medium: 0.003% Polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 50 rpm, with sinkers

Times: 2 h for the Acid stage medium, and 3 and 5 h for the Buffer stage medium (including the 2 h in the Acid stage medium)

Buffer solution: Dissolve 1.0 g of octanesulfonic acid sodium salt and 1.4 g of monobasic potassium phosphate in 1 L of water. Adjust with potassium hydroxide to a pH of 6.5 ± 0.05.

Mobile phase: Buffer solution and acetonitrile (3:2)

Standard stock solution: 0.04 mg/mL of USP Tamsulosin Hydrochloride RS in Buffer stage medium

Standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of 0.8 μg/mL.

Sample solution: Centrifuge a portion of the solution under test at NMT 3000 rpm for NLT 20 min.

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 1 and 3 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 3.9-mm × 7.5-cm; 5-μm packing L7

Column temperature: 30°

Flow rate: 1.5 mL/min

Injection volume: 100 μL

System suitability

Sample: Standard solution

Suitability requirements

Relative standard deviation: NMT 4.0%

Analysis

Samples: Standard solution and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (μg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium, mL

Tolerances: See Table 5.

Table 5

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 6: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 6.

Acid stage medium: 0.003% Polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 100 rpm using a 40-mesh basket as a sinker, and the paddle height adjusted at 4.5 cm from the bottom of the vessel

Times: 2 h for the Acid stage medium, and 3 and 8 h for the Buffer stage medium (including the 2 h in the Acid stage medium)

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 1 and 6 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed.

Buffer solution: Dissolve 3 g of sodium hydroxide and 8.7 mL of perchloric acid in 1900 mL of water, adjust with 0.5 M sodium hydroxide to a pH of 2.0 ± 0.05, and dilute with water to 2000 mL.

Mobile phase: Buffer solution and acetonitrile (7:3)

Standard stock solution: 0.5 mg/mL of USP Tamsulosin Hydrochloride RS in methanol

Acid stage standard solution: Dilute the Standard stock solution with Acid stage medium to obtain a final concentration of 0.8 μg/mL.

Buffer stage standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of 0.8 μg/mL.

Sample solution: Pass a portion of the solution under test through a suitable fIlter of 0.45-μm pore size.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 4.6-mm × 15-cm, 3-μm packing L1

Column temperature: 40°

Flow rate: 1.5 mL/min

Injection volume: 100 μL

System suitability

Samples: Acid stage standard solution and Buffer stage standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

Analysis

Samples: Acid stage standard solution, Buffer stage standard solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the appropriate Standard solution

C_S = concentration of the appropriate Standard solution (μg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium, mL

Tolerances: See Table 6.

Table 6

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 7: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 7.

Acid stage medium: 0.003% polysorbate 80, in pH 1.2 simulated gastric fluid without enzyme (prepare a solution containing 3.00 g of polysorbate 80 in 200 mL of water, and dilute 2 mL of this solution to 1 L with simulated gastric fluid without enzyme); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL, deaerated

Apparatus 2: 100 rpm, with wire helix sinkers

Times: 2 h in the Acid stage medium, and 4 and 12 h in the Buffer stage medium (including the 2 h in the Acid stage medium)

Solution A: 2.76 g/L of monobasic sodium phosphate monohydrate in water. Adjust with phosphoric acid to a pH of 2.5 ± 0.05.

Solution B: Acetonitrile

Mobile phase: See Table 7.

Table 7

Table 7

Standard stock solution: 1 mg/mL of USP Tamsulosin Hydrochloride RS in alcohol

Acid stage standard solution: Dilute the Standard stock solution with Acid stage medium to obtain a final concentration of about 0.2 μg/mL.

Buffer stage standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of about 0.8 μg/mL.

Sample solution: Pass a portion of the solution under test through a suitable fIlter of 0.45-μm pore size.

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 2 and 10 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 2-mm × 5-cm; packing L1

Column temperature: 30°

Flow rate: 1.5 mL/min

Injection volume: 100 μL

System suitability

Samples: Acid stage standard solution and Buffer stage standard solution

Suitability requirements

Tailing factor: NMT 1.5

Relative standard deviation: NMT 2.0%

Analysis

Samples: Acid stage standard solution, Buffer stage standard solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the appropriate Standard solution

C_S = concentration of the appropriate Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium, mL

Tolerances: See Table 8.

Table 8

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 8: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 8.

Acid stage medium: 0.003% polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 100 rpm, with sinkers

Times: 2 h in the Acid stage medium, and 3 and 8 h in the Buffer stage medium (including the 2 h in the Acid stage medium)

Standard stock solution: 0.4 mg/mL of USP Tamsulosin Hydrochloride RS in methanol

Acid stage standard solution: Dilute the Standard stock solution with Acid stage medium to obtain a final concentration of 0.8 μg/mL.

Buffer stage standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of 0.8 μg/mL.

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 1 and 6 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed.

Sample solution: Pass a portion of the solution under test through a suitable fIlter of 0.45-μm pore size.

Buffer solution: Dissolve 6.8 g of dibasic ammonium phosphate in 800 mL of water, and add 2 mL of triethylamine. Adjust with phosphoric acid to a pH of 6.5. Dilute with water to 1000 mL.

Mobile phase: Buffer solution and acetonitrile (7:3)

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 4.6-mm × 15-cm; 5-μm packing L1

Column temperature: 30°

Flow rate: 1.0 mL/min

Injection volume: 100 μL

System suitability

Sample: Buffer stage standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

Analysis

Samples: Acid stage standard solution, Buffer stage standard solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response of tamsulosin from the Sample solution

r_S = peak response of tamsulosin from the appropriate Standard solution

C_S = concentration of the appropriate Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium, mL

Tolerances: See Table 9.

Table 9

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 9: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 9.

Acid stage medium: 0.003% polysorbate 80, pH 1.2 (proceed as directed for Test 2); 500 mL

Buffer stage medium: pH 7.2 phosphate buffer (proceed as directed for Test 1); 500 mL

Apparatus 2: 100 rpm, with helix wire coil sinker

Times: 2 h in Acid stage medium, and 3 and 8 h in Buffer stage medium (including the 2 h in Acid stage medium)

Standard stock solution: 0.05 mg/mL of USP Tamsulosin Hydrochloride RS in methanol

Acid stage standard solution: Dilute the Standard stock solution with Acid stage medium to obtain a final concentration of 0.8 μg/mL.

Buffer stage standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of 0.8 μg/mL.

Sample solution: Pass a portion of the solution under test through a suitable fIlter of 0.45-μm pore size.

Procedure: Perform the test using the Acid stage medium. At 2 h after the start of the test, withdraw a sample of the solution under test.

Carefully discard the Acid stage medium, replace it with the Buffer stage medium previously warmed, and continue the test. At 1 and 6 h after the replacement of the medium, withdraw a sample of the solution under test. Replace the volume of medium withdrawn with the same volume of Buffer stage medium, previously warmed.

Buffer: 3.45 g/L of monobasic ammonium phosphate in water. Adjust with triethylamine to a pH of 6.5 ± 0.05.

Mobile phase: Buffer and acetonitrile (3:2). Add 1 g of sodium 1-pentanesulfonate per liter of the mixture.

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 4.6-mm × 25-cm; 5-μm packing L7

Flow rate: 1 mL/min

Injection volume: 100 μL

System suitability

Samples: Acid stage standard solution or Buffer stage standard solution

Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 2.0%

Analysis

Samples: Acid stage standard solution, Buffer standard solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response from the Sample solution

r_S = peak response from the appropriate Standard solution

C_S = concentration of the appropriate Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the speciFIed time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V_S = volume of the Buffer stage medium, 500 mL

V₂ = volume of the Sample solution withdrawn and replaced with medium, mL

Tolerances: See Table 10.

Table 10

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Test 10: If the product complies with this test, the labeling indicates that it meets USP Dissolution Test 10.

Acid stage medium: Dissolve 2.0 g of sodium chloride and 5.7 mL of hydrochloric acid in 1000 mL of water. To 500 mL of this solution add 1 mL of polysorbate 80 aqueous solution (3 g in 200 mL of water) just before the test; 500 mL.

Buffer stage medium: pH 7.2 phosphate buffer (dissolve 68 g of monobasic potassium phosphate and 13.8 g of sodium hydroxide in 10 L of water, and adjust with dilute sodium hydroxide solution or dilute phosphoric acid to a pH of 7.2); 500 mL

Apparatus 2: 100 rpm, with a suitable sinker

Times: 2, 3, and 8 h

Procedure: Perform the test using Acid stage medium. At 2 h after the start of the test, withdraw 10.0 mL of the solution under test. Drain the Acid stage medium immediately using a 60-mesh stainless wire screen. Add the Buffer stage medium previously warmed, and continue the test. At 3 h after the start of the test (1 h after replacement of the medium), withdraw 10.0 mL of the solution under test, replace the same volume with warmed Buffer stage medium, and continue the test. At 8 h after the start of the test (6 h after the replacement of the medium), withdraw 10.0 mL of the solution under test.

Standard stock solution: Prepare a solution containing 0.5 mg/mL of USP Tamsulosin Hydrochloride RS in acetonitrile and water (3:7).

Acid stage standard solution: Dilute the Standard stock solution with Acid stage medium to obtain a final concentration of about 0.8 μg/mL.

Buffer stage standard solution: Dilute the Standard stock solution with Buffer stage medium to obtain a final concentration of about 0.8 μg/mL.

Sample solution: Pass a portion of the solution under test through a suitable glass fiber fIlter, discarding the first 5 mL of the filtrate.

Chromatographic system: Proceed as directed in the Assay, Procedure 10 except for Injection volume.

Injection volume: 100 μL

System suitability

Samples: Acid stage standard solution and Buffer stage standard solution

Suitability requirements

Relative standard deviation: NMT 2.0%

Analysis

Samples: Acid stage standard solution, Buffer stage standard solution, and Sample solution

Calculate the concentration (C_i ) of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the sample withdrawn from the vessel at each time point (i):

Result_i = (r_U /r_S ) × C_S

r_U = peak response from the Sample solution

r_S = peak response from the appropriate Standard solution

C_S = concentration of the appropriate Standard solution (mg/mL)

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at each time point (i):

Result₁ = C₁ × V₁ × (1/L) × 100

Result₂ = [C₂ × V₂ × (1/L) × 100] + Result₁

Result₃ = {[(C₃ × V₂ ) + (C₂ × V_S)] × (1/L) × 100} + Result₁

C_i = concentration of tamsulosin hydrochloride in the portion of sample withdrawn at the specified time point (mg/mL)

V₁ = volume of the Acid stage medium, 500 mL

L = label claim (mg/Capsule)

V₂ = volume of the Buffer stage medium, 500 mL

V_S = volume of the Sample solution withdrawn and replaced with medium, 10 mL

Tolerances: See Table 11.

Table 11

The percentages of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) dissolved at the times specified conform to

Dissolution 〈711〉, Acceptance Table 2.

Uniformity of Dosage Units 〈905〉: Meet the requirements

Procedure for content uniformity

[Note—Use the following Procedure for content uniformity if Procedure 1 is used in the Assay. For all other formulations, proceed as directed in

Uniformity of Dosage Units 〈905〉.]

Solution A, Solution B, Mobile phase, and Standard stock solution: Prepare as directed in the Assay, Procedure 1.

Internal standard solution: 0.16 mg/mL of propylparaben in a mixture of acetonitrile and water (3:7)

Standard stock solution 1: Transfer 5.0 mL of the Standard stock solution to a 25-mL volumetric flask, and dilute with a mixture of acetonitrile and water (3:7) to volume.

Standard solution: Transfer 4.0 mL of Standard stock solution 1 to a suitable container. Add 5.0 mL of the Internal standard solution, and add the Mobile phase to make 40 mL.

Sample solution: Place the contents of 1 Capsule into a Teflon-lined, screw-capped centrifuge tube. Place approximately 100 glass balls with a diameter of about 5 mm into the tube, add 20 mL of 0.05 N sodium hydroxide, heat at 50° for 10 min, and shake well for 30 min.

Add 15 mL of a mixture of acetonitrile and Solution A (2:1) to the solution, and shake well. Add 5.0 mL of the Internal standard solution, and shake well. Centrifuge at 1500 rpm for 10 min, and use the supernatant, passing it if necessary through a membrane fIlter of 0.5-μm or smaller pore size.

Chromatographic system: Proceed as directed in the Assay, Procedure 1 except for Injection volume.

Injection volume: 25 μL

Analysis

Samples: Standard stock solution 1, Standard solution, and Sample solution

Calculate the percentage of the labeled amount of tamsulosin hydrochloride (C₂₀H₂₈N₂O₅S · HCl) in the Capsules taken:

Result = (R_U /R_S ) × [C_S × (V_S /L)] × 100

R_U = peak area ratio of tamsulosin to the internal standard from the Sample solution

R_S = peak area ratio of tamsulosin to the internal standard from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in Standard stock solution 1 (mg/mL)

V_S = volume of Standard stock solution 1 taken to prepare the Standard solution (mL)

L = label claim (mg/Capsule)

5 IMPURITIES

Organic Impurities

Buffer: 1.5 g/L of sodium hydroxide and 4.4 mL/L of perchloric acid in water. Adjust with 0.5 M sodium hydroxide or dilute perchloric acid to a

pH of 2.0 and dilute with water to volume.

Solution A: 4.3 g/L of octanesulfonic acid sodium and 13.3 g/L monobasic sodium phosphate in water. Adjust with phosphoric acid to a pH of 3.0.

Solution B: Methanol and acetonitrile (70:30)

Mobile phase: See Table 12.

Table 12

Diluent 1: 0.1 N sodium hydroxide

Diluent 2: Buffer and acetonitrile (70:30)

Standard stock solution: 0.8 mg/mL of USP Tamsulosin Hydrochloride RS prepared as follows. Transfer 40 mg of USP Tamsulosin

Hydrochloride RS to a 50-mL volumetric flask and add 5 mL of Diluent 1 and 30 mL of Diluent 2. Sonicate to dissolve and dilute with Diluent 2 to volume.

Standard solution: 0.8 μg/mL of USP Tamsulosin Hydrochloride RS from the Standard stock solution in Diluent 2

Sensitivity solution: 0.08 μg/mL of USP Tamsulosin Hydrochloride RS from the Standard solution in Diluent 2

Sample solution: Nominally 80 μg/mL of tamsulosin hydrochloride prepared as follows. Calculate the average fill weight of NLT 20 Capsules and homogenize. Transfer 4 mg of tamsulosin hydrochloride to a 50-mL volumetric flask, add 10 mL of Diluent 1, and stir for NLT 15 min with a magnetic stirring bar. To this mixture add 20 mL of Diluent 2 and continue stirring for NLT 15 min ensuring complete dispersion of pellets. Remove the magnetic stirring bar, rinse with Diluent 2, and sonicate with intermittent shaking for NLT 25 min. Allow the solution to cool to room temperature and dilute with Diluent 2 to volume. Centrifuge the solution for NLT 10 min and fIlter the supernatant through a suitable 0.45-μm pore size fIlter. [Note—The use of a centrifuge speed of 3000 rpm may be suitable.]

Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 225 nm

Column: 4.6-mm × 15-cm; 5-μm packing L1

Column temperature: 50°

Flow rate: 1 mL/min

Injection volume: 50 μL

System suitability

Samples: Standard solution and Sensitivity solution

[Note—The relative retention times for methoxy tamsulosin, tamsulosin, ethoxyphenoxy ethyl bromide, and desethoxy tamsulosin are 0.73,

1.00, 1.80, and 2.80, respectively.]

Suitability requirements

Tailing factor: NMT 2.0, Standard solution

Relative standard deviation: NMT 5.0%, Standard solution

Signal-to-noise ratio: NLT 10, Sensitivity solution

Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of any individual impurity in the portion of Capsules taken:

Result = (r_U/r_S) × (C_S /C_U ) × (1/F) × 100

r_U = peak response of any individual impurity from the Sample solution

r_S = peak response of tamsulosin from the Standard solution

C_S = concentration of USP Tamsulosin Hydrochloride RS in the Standard solution (μg/mL)

C_U = nominal concentration of tamsulosin hydrochloride in the Sample solution (μg/mL)

F = relative response factor (see Table 13)

Acceptance criteria: See Table 13. The reporting threshold is 0.1%.

Table 13

^a (R)-5-(2-Aminopropyl)-2-methoxybenzenesulfonamide.

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight containers. Store at controlled room temperature.

Labeling: When more than one Dissolution test is given, the labeling states the Dissolution test used only if Test 1 is not used.

USP Reference Standards 〈11〉

USP Tamsulosin Hydrochloride RS