JP XVI Official Monographs / Sodium Pyrosulfite 1411

50 mL. Perform the test using this solution as the test solu- Sodium Hydrate tion. Prepare the control solution as follows: to 0.40 mL of 0.005 mol/L sulfuric acid VS add 20 mL of acetone, 1 mL of プラステロン硫酸エステルナトリウム水和物 dilute hydrochloric acid and water to make 50 mL (not more than 0.032z). (4) Heavy metals <1.07>—Proceed with 2.0 g of Sodium Prasterone Sulfate Hydrate according to Method 2, and per- form the test. Prepare the control solution with 2.0 mL of Standard Lead Solution (not more than 10 ppm). (5) Related substances—Dissolve 0.10 g of Sodium Prasterone Sulfate Hydrate in 10 mL of methanol, and use

C19H27NaO5S.2H2O: 426.50 this solution as the sample solution. Pipet 1 mL of the sam- Monosodium 17-oxoandrost-5-en-3b-yl sulfate dihydrate ple solution, add methanol to make exactly 200 mL, and use [1099-87-2, anhydride] this solution as the standard solution. Perform the test with these solutions as directed under Thin-layer Chromatogra- Sodium Prasterone Sulfate Hydrate contains not phy <2.03>. Spot 5 mL each of the sample solution and stand- less than 98.0z of sodium prasterone sulfate ard solution on a plate of silica gel with fluorescent indicator (C19H27NaO5S: 390.47), calculated on the dried basis. for thin-layer chromatography. Develop the plate with a mixture of , methanol and water (75:22:3) to a Description Sodium Prasterone Sulfate Hydrate occurs as distance of about 10 cm, and air-dry the plate. Spray evenly white crystals or crystalline powder. It is odorless. a mixture of sulfuric acid and ethanol (95) (1:1) on the plate, It is soluble in methanol, sparingly soluble in water and in and heat at 809C for 5 minutes: the spots other than the ethanol (95), and practically insoluble in acetone and in principal spot from the sample solution are not more intense . than the spot from the standard solution. The pH of a solution of Sodium Prasterone Sulfate Hy- drate (1 in 200) is between 4.5 and 6.5. Loss on drying <2.41> 8.0–9.0z (0.5 g, in vacuum, phos- Melting point: about 1609C (with decomposition, after phorus (V) oxide, 609C, 3 hours). drying). Assay Weigh accurately about 0.25 g of Sodium Praster- Identification (1) Dissolve 0.01 g of Sodium Prasterone one Sulfate Hydrate, dissolve in 30 mL of water. Apply this Sulfate Hydrate in 4 mL of ethanol (95), add 2 mL of 1,3- solution to a chromatographic column 10 mm in inside di- dinitrobenzene TS and 2 mL of a solution of sodium hydrox- ameter, previously prepared by pouring 5 mL of strongly ide (1 in 8): a red-purple color develops, and gradually acidic -exchange resin (H type) for column chromatogra- changes to brown. phy, and elute at the rate of 4 mL per minute. Wash the (2) To 10 mL of a solution of Sodium Prasterone Sulfate chromatographic column with 100 mL of water, combine the Hydrate (1 in 200) add 0.5 mL of bromine TS: the color of washings with above effluent solution, and titrate <2.50> bromine TS immediately disappears. with 0.05 mol/L sodium hydroxide VS (potentiometric titra- (3) Determine the infrared absorption spectrum of So- tion). Perform a blank determination, and make any neces- dium Prasterone Sulfate Hydrate as directed in the potas- sary correction. sium disk method under the Infrared Spectro- Each mL of 0.05 mol/L sodium hydroxide VS photometry <2.25>, and compare the spectrum with the ＝ 19.52 mg of C H NaO S Reference Spectrum: both spectra exhibit similar intensities 19 27 5 of absorption at the same wave numbers. Containers and storage Containers—Tight containers. (4) A solution of Sodium Prasterone Sulfate Hydrate (1 in 200) responds to the Qualitative Tests <1.09> for sodium salt. Sodium Pyrosulfite 20 Optical rotation <2.49> [a]D : ＋10.7 – ＋12.19(0.73 g, cal- culated on the dried basis, methanol, 20 mL, 100 mm). Sodium Metabisulfite Purity (1) Clarity and color of solution—Dissolve 0.25 g ピロ亜硫酸ナトリウム of Sodium Prasterone Sulfate Hydrate in 50 mL of water: the solution is clear and colorless. Na S O : 190.11 (2) Chloride <1.03>—Dissolve 1.0 g of Sodium Praster- 2 2 5 one Sulfate Hydrate in 20 mL of acetone and 20 mL of Sodium Pyrosulfite contains not less than 95.0z of water, and add 6 mL of dilute nitric acid and water to make Na S O . 50 mL. Perform the test using this solution as the test solu- 2 2 5 tion. Prepare the control solution as follows: to 0.30 mL of Description Sodium Pyrosulfite occurs as white crystals or 0.01 mol/L hydrochloric acid VS add 20 mL of acetone, 6 crystalline powder. It has the odor of sulfur dioxide. mL of dilute nitric acid and water to make 50 mL (not more It is freely soluble in water, very slightly soluble in ethanol than 0.011z). (95), and practically insoluble in diethyl ether. (3) Sulfate <1.14>—To 1.2 g of Sodium Prasterone Sul- A solution of Sodium Pyrosulfite (1 in 20) is acid. fate Hydrate add 20 mL of water, shake vigorously for 5 It is hygroscopic. minutes, and filter. To 10 mL of the filtrate add 20 mL of It decomposes slowly on exposure to air. acetone, 1 mL of dilute hydrochloric acid and water to make