Sodium Picosulfate

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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C₁₈H₁₃NNa₂O₈S₂ · H₂O 499.42

4,4′-(2-Pyridylmethylene)diphenyl bis(hydrogen sulfate) disodium salt, monohydrate;

Sodium 4,4’-(Pyridin-2-ylmethylene)bis(4,1-phenylene) disulfate monohydrate CAS RN®: 1307301-38-7; UNII: LR57574HN8. (USP 1-Aug- 2023)

Anhydrous

C₁₈H₁₃NNa₂O₈S₂ 481.40 (USP 1-Aug-2023) CAS RN®: 10040-45-6; UNII: VW106606Y8.

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1 DEFINITION

Sodium Picosulfate contains NLT 98.0% (USP 1-Aug-2023) and NMT 102.0% (USP 1-Aug-2023) of sodium picosulfate (C₁₈H₁₃NNa₂O₈S₂), calculated on the anhydrous basis.

2 IDENTIFICATION

A. Spectroscopic Identification Tests 〈197〉, Infrared Spectroscopy: 197A, 197K, or 197M

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B. Identification Tests—General 〈191〉, Chemical Identification Tests, (USP 1-Aug-2023) Sodium: Meets the requirements

(USP 1-Aug-2023)

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C. The retention time of the major peak of the Sample solution corresponds to that of the Standard solution, as obtained in the Assay. (USP 1-Aug-2023)

3 ASSAY

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3.1 Procedure

Buffer: 2.3 g/L of dibasic sodium phosphate dihydrate in water. To each liter of solution, add 200 mg of cetyltrimethylammonium bromide, and adjust with phosphoric acid to a pH of 7.5.

Mobile phase: Acetonitrile and Buffer (45:55)

[Note—If necessary, vary the buffer/acetonitrile proportion in 10-mL increments per liter of Mobile phase in order to fulfill the resolution requirement.]

Standard solution: 0.05 mg/mL of USP Sodium Picosulfate RS in Mobile phase

Sample solution: 0.05 mg/mL of Sodium Picosulfate in Mobile phase

3.2 Chromatographic system

(See Chromatography 〈621〉, System Suitability.)

Mode: LC

Detector: UV 263 nm

Column: 4.6-mm × 25-cm; 5-μm packing L1

Column temperature: 40°

Flow rate: 1 mL/min

Injection volume: 40 μL

Run time: NLT 2 times the retention time of sodium picosulfate

3.3 System suitability

Sample: Standard solution

3.4 Suitability requirements

Tailing factor: NMT 2.0

Relative standard deviation: NMT 0.73%

3.5 Analysis

Samples: Standard solution and Sample solution

Calculate the percentage of sodium picosulfate in the portion of Sodium Picosulfate taken:

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

r_U = peak response of sodium picosulfate from the Sample solution

r_S = peak response of sodium picosulfate from the Standard solution

C_S = concentration of USP Sodium Picosulfate RS in the Standard solution (mg/mL)

C_U = concentration of Sodium Picosulfate in the Sample solution (mg/mL)

(USP 1-Aug-2023)

Acceptance criteria: 98.0%–102.0% (USP 1-Aug-2023) on the anhydrous basis

4 IMPURITIES

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Chloride and Sulfate 〈221〉, Chloride

Sample: 1.0 g

Acceptance criteria: The turbidity in the Sample does not exceed that produced in (USP 1-Aug-2023) 0.30 mL of 0.020 N hydrochloric acid (NMT 0.02%).

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Chloride and Sulfate 〈221〉, Sulfate

Sample: 500 mg

Acceptance criteria: The turbidity in the Sample does not exceed that produced in (USP 1-Aug-2023) 0.20 mL of 0.020 N sulfuric acid (NMT 0.04%).

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Organic Impurities Buffer, Mobile phase, and Chromatographic system: Proceed as directed in the Assay. (USP 1-Aug-2023)

System suitability solution: 0.5 mg/mL of USP Sodium Picosulfate RS (USP 1-Aug-2023) and 0.5 μg/mL of USP Sodium Picosulfate Related

Compound A RS

(USP 1-Aug-2023) , in Mobile phase

Standard solution: (USP 1-Aug-2023) 0.5 μg/mL of USP Sodium Picosulfate RS (USP 1-Aug-2023) in Mobile phase

(USP 1-Aug-2023)

Sensitivity solution: 0.25 μg/mL of USP Sodium Picosulfate RS from the Standard solution, (USP 1-Aug-2023) in Mobile phase

(USP 1-Aug- 2023)

Sample solution: 500 μg/mL (USP 1-Aug-2023) of Sodium Picosulfate in Mobile phase

(USP 1-Aug-2023)

System suitability

Samples: System suitability solution, Standard solution, (USP 1-Aug-2023) and Sensitivity solution

Suitability requirements

Resolution: NLT 4 between sodium picosulfate related compound A and sodium picosulfate, System suitability solution

Relative standard deviation: NMT 5.0%, Standard solution (USP 1-Aug-2023)

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

Analysis

Samples: Sample solution and Standard solution (USP 1-Aug-2023)

Calculate the percentage of any impurity in the portion of Sodium Picosulfate taken:

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

r_U = peak response of any impurity from the Sample solution

r_S = peak response of sodium picosulfate from the Standard solution (USP 1-Aug-2023)

C_S = concentration of USP Sodium Picosulfate RS (USP 1-Aug-2023) in the Standard solution (μg/mL) (USP 1-Aug-2023)

C_U = concentration of Sodium Picosulfate in the Sample solution (μg/mL (USP 1-Aug-2023) )

F = relative response factor (see Table 1)

Acceptance criteria: See Table 1. The reporting threshold is (USP 1-Aug-2023) 0.05%.

Table 1

^a 4,4'-(Pyridin-2-ylmethylene)diphenol.

5 SPECIFIC TESTS

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Color of Solution (USP 1-Aug-2023)

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Acidity and Alkalinity (USP 1-Aug-2023)

Water Determination 〈921〉, Method I, Method Ia: 3.0%–5.0%

6 ADDITIONAL REQUIREMENTS

Packaging and Storage: Preserve in tight, light-resistant containers. Store at room temperature.

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USP Reference Standards 〈11〉

USP Sodium Picosulfate RS

USP Sodium Picosulfate Related Compound A RS

Sodium 4-((4-hydroxyphenyl)(pyridin-2-yl)methyl)phenyl sulfate. (USP 1-Aug-2023)

C₁₈H₁₄NNaO₅S   379.36