USP 35 Official Monographs / Aurothioglucose 2273

atropine sulfate [(C 17H23NO3)2 · H2SO4 · H2O] in the portion of Loss on ignition ⟨733⟩—When ignited at 1000 ° for 1 hour, itTablets taken by the formula: loses between 17.0% and 27.0% of its weight.

Volatile matter—When ignited at 600 ° for 1 hour, it loses(694.85 / 676.83)(W / 10)(RU / RS) between 7.5% and 12.5% of its weight on the dried basis.

Powder fineness—Add 50 g to 450 mL of water containingin which 694.85 and 676.83 are the molecular weights of atro- 5 g of sodium pyrophosphate, and stir for 10 minutes. Pour thepine sulfate monohydrate and anhydrous atropine sulfate, re- resulting dispersion slowly through a No. 325 standard sievespectively; W is the weight, in mg, of USP Atropine Sulfate RS (see Particle Size Distribution Estimation by Analytical Sievingin the Standard preparation; and RU and RS are as defined ⟨786⟩), and carefully wash the residue until clean. Dr y the resi-therein. due at 105 ° to constant weight: the dr y weight of the residueso obtained is not more than 0.30% of the weight of the speci-men taken.

. Acid-soluble matter—Boil 2.0 g with 100 mL of 0.2 N hy-drochloric acid for 5 minutes, and cool. Add water to adjust theActivated Attapulgitevolume to 100 mL, and filter. Evaporate 50 mL of the filtrate soobtained to dryness, and ignite the residue at 600 °: not more» Activated Attapulgite is a highly heat-treated,than 0.15 g is found (15%).processed, native magnesium aluminum silicate.Carbonate—Mix 1.0 g with 15 mL of 0.5 N sulfuric acid: noeffervescence occurs.Packaging and storage—Preserve in well-closed containers.Arsenic and Lead—To 5.0 g add 50 mL of 1 N nitric acid,Identification—Activated Attapulgite responds to the Identifi-and boil for 30 minutes, adding 1 N nitric acid at times tocation test for Colloidal Activated Attapulgite, the characteristicmaintain the volume. Filter into a 100-mL volumetric flask,peak, however, being much less intense.wash the filter with water, and dilute the combined filtrate andLoss on drying ⟨731⟩—Dry it at 105 ° to constant weight: itwashings with water to volume.loses not more than 4.0% of its weight.

Arsenic—Determine the arsenic in the solution by atomic ab-Loss on ignition ⟨733⟩—When ignited at 1000 ° for 1 hour, itsorption spectrometry (see Spectrophotometry and Light-scatter-loses between 4.0% and 12.0% of its weight.ing ⟨851⟩), using a graphite furnace to volatilize the arsenic, asVolatile matter—When ignited at 600 ° for 1 hour, it loses directed by the manufacturer of the instrument used, andbetween 3.0% and 7.5% of its weight on the dried basis. measuring the absorbance at 189.0 nm against a standard: not

Powder fineness—Proceed as directed in the test for Powder more than 2 ppm is found.fineness under Colloidal Activated Attapulgite. The dry weight of Lead—Determine the lead in the solution by atomic absorp-the residue is not more than 0.10% of the weight of the speci- tion spectrometry (see Spectrophotometry and Light-scatteringmen taken. ⟨851⟩), using a graphite furnace to volatilize the lead, as di-Acid-soluble matter—Boil 2.0 g with 100 mL of 0.2 N hy- rected by the manufacturer of the instrument used, and meas-drochloric acid for 5 minutes, and cool. Add water to adjust the uring the absorbance at 283.3 nm against a standard: not morevolume to 100 mL, and filter. Evaporate 50 mL of the filtrate so than 0.001% is found.obtained to dryness, and ignite the residue at 600 °: not more Adsorptive capacity—To 10 mL of a 1 in 10 suspension ofthan 0.25 g is found (25%). the specimen in water add 80 mL of methylene blue solution (1Other requirements—It meets the requirements of the tests in 1000), and shake. Add 10 mL of barium chloride solution (1for Microbial limits, pH, Carbonate, Arsenic and Lead, and Adsorp- in 50), and shake. Allow to stand for 15 minutes. T ransfer 40tive capacity under Colloidal Activated Attapulgite. mL of the supernatant to a 50-mL centrifuge tube, and centri-

fuge. To 5 mL of the clear supernatant add 495 mL of water,and mix: the color of the solution so obtained is not deeperthan that of a solution containing 1.5 µg of methylene blue per

. mL.Colloidal Activated Attapulgite

» Colloidal Activated Attapulgite is a purified na-.tive magnesium aluminum silicate. Aurothioglucose

Packaging and storage—Preserve in well-closed containers.Identification—Add 2 g in small portions to 100 mL of water,with vigorous agitation. Allow to stand for at least 12 hours toensure complete hydration. Place 2 mL of the resulting mixtureon a suitable glass slide, and allow to air-dr y at room tempera-ture to produce a uniform film. Place the slide in a vacuumdesiccator over a free sur face of ethylene glycol. Evacuate the C6H11AuO5S 392.18desiccator, and close the stopcock so that the ethylene glycol Gold, (1-thio-D-glucopyranosato)-.saturates the desiccator chamber. Allow to stand for 12 hours. (1-Thio-D-glucopyranosato)gold [12192-57-3].Record the X-ray diffraction pattern (see X-Ray Diffraction⟨941⟩), and calculate the d values: several peaks are obser ved; » Aurothioglucose contains not less than 95.0the characteristic peak corresponds to a d value between 10.3 percent and not more than 105.0 per cent ofand 10.7 Angstrom units.

C6H11AuO5S, calculated on the dried basis. It isMicrobial enumeration tests ⟨61⟩ and Tests for specifiedstabilized by the addition of a small amount ofmicroorganisms ⟨62⟩—It meets the requirements of the test

for absence of Escherichia coli. Sodium Acetate.pH ⟨791⟩—Disperse 1.0 g in 10 mL of carbon dioxide-free

Packaging and storage—Preserve in tight, light-resistantwater, and mix: the pH of the mixed dispersion so obtained iscontainers. Store at room temperature.between 7.0 and 9.5.

Loss on drying ⟨731⟩—Dry it at 105 ° to constant weight: it USP Reference standards ⟨11⟩—loses between 5.0% and 17.0% of its weight. USP Aurothioglucose RS

Official from May 1, 2012Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.

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2274 Aurothioglucose / Official Monographs USP 35

Identification— tone, then transfer the filter and its contents to a short-necked,300-mL Kjeldahl flask, add 5 mL of water, and proceed as di-A: Dissolve a suitable quantity in water to obtain a solutionrected in the Assay under Gold Sodium Thiomalate, beginningcontaining 4 mg per mL. Apply 10 µL of this solution and 10with “add 20 mL of nitric acid.” The weight of gold so ob-µL of an aqueous Standard solution of USP Aurothioglucose RStained, multiplied by 1.991, represents the weight ofcontaining 4 mg per mL to a suitable thin-layer chromato-C6H11AuO5S in the portion of Injectable Suspension taken.graphic glass microfilament sheet (see Chromatography ⟨621⟩)

impregnated with silicic acid and a suitable fluorescing sub-stance. Allow the spots to dr y, and develop the chromatogramin a solvent system consisting of a mixture of n-propyl alcohol,

.water, and ethyl acetate (3:3:1) until the solvent front has Avobenzonemoved about three-fourths of the length of the plate. Removethe sheet from the developing chamber, mark the solvent front,and allow the solvent to evaporate. Locate the spots on theplate by examination under short-wavelength UV light: the RF

value of the principal spot obtained from the solution undertest corresponds to that obtained from the Standard solution.

B: To a portion of the filtrate obtained in the Assay addbarium chloride TS: a heavy, white precipitate is formed. C20H22O3 310.40

1,3-Propanedione, 1-[4-(1,1-dimethylethyl)phenyl]-3-(4-methox-Specific rotation ⟨781S⟩: between +65° and +75 °.yphenyl)-.Test solution: 10 mg per mL, in water. 1-(p-tert-Butylphenyl)-3-(p-methoxyphenyl)-1,3-propanedione

Loss on drying ⟨731⟩—Dry it over phosphorus pentoxide for [70356-09-1].24 hours: it loses not more than 1.0% of its weight.Assay—Accurately weigh about 1 g of Aurothioglucose, and » Avobenzone contains not less than 95.0 per-dissolve in 100 mL of water in a 300-mL Kjeldahl flask. Slowly cent and not more than 105.0 per cent ofadd 10 mL of nitric acid, and when the reaction has subsided, C20H22O3, calculated on the dried basis.boil the mixture for 5 minutes. Filter, wash well the separatedgold with hot water, dr y, and ignite to constant weight. The Packaging and storage—Preserve in tight, light-resistantweight of the gold so obtained, multiplied by 1.991, represents containers.the weight of C 6H11AuO5S in the portion of Aurothioglucosetaken. USP Reference standards ⟨11⟩—

USP Avobenzone RSIdentification—

A: Infrared Absorption ⟨197K⟩..

B: Ultraviolet Absorption ⟨197U⟩—Aurothioglucose Injectable SuspensionSolution: 5 µg per mL.

» Aurothioglucose Injectable Suspension is a ster- Medium: alcohol.Absorptivities at 360 nm do not differ by more than 3.0%.ile suspension of Aurothioglucose in a suitable

Melting range, Class I ⟨741⟩: between 81° and 86 °.vegetable oil. It contains not less than 90.0 per-Loss on drying ⟨731⟩—Dry it in vacuum at 70 ° for 4 hours: itcent and not more than 110.0 per cent of theloses not more than 0.5% of its weight.labeled amount of C 6H11AuO5S. It may containChromatographic purity—suitable thickening agents.

Test solution—Proceed as directed for Assay preparation inPackaging and storage—Preserve in single-dose or in multi- the Assay.ple-dose containers, preferably of T ype I glass. Protect from Chromatographic system (see Chromatography ⟨621⟩)—Pro-light. ceed as directed in the Assay.

Procedure—Inject a volume (about 1 µL) of Test solution intoUSP Reference standards ⟨11⟩—the chromatograph, record the chromatogram, and measureUSP Aurothioglucose RSthe peak responses. Calculate the per centage of each impurityIdentification—Transfer a volume of Injectable Suspension, in the portion of A vobenzone taken by the formula:equivalent to about 200 mg of aurothioglucose, to a centrifuge

separator containing 20 mL of ethyl acetate and 50 mL of 100(rI / rS)water. Shake the mixture thoroughly, and centrifuge until theliquid phases have been clearly separated. W ithdraw the lower, in which rI is the response of each individual peak, other thanaqueous phase, and filter, discarding the first 10 mL of the the avobenzone peak, in the chromatogram of the Test solution;filtrate. Collect the filtrate in a glass-stoppered vessel, and pro- and rS is the sum of the responses of all of the peaks in theceed as directed in Identification test A under Aurothioglucose, chromatogram of the Test solution: not more than 3.0% of anybeginning with “apply 10 µL of this solution.” individual impurity is found, and the sum of all of the impuritiesBacterial endotoxins ⟨85⟩—It contains not more than 7.14 is not more than 4.5%.USP Endotoxin Units per mg of aurothioglucose. Assay—Sterility ⟨71⟩—It meets the requirements. Standard preparation—Dilute an accurately measured quan-Other requirements—It meets the requirements under Injec- tity of USP A vobenzone RS in acetone, and dilute quantitatively,tions ⟨1⟩. and stepwise if necessar y, with acetone to obtain a solution

having a known concentration of about 50 mg per mL.Assay—Transfer with a pipet, calibrated to contain rather thanto deliver, an accurately measured volume of Injectable Suspen- Assay preparation—Transfer about 500 mg of A vobenzone,sion, equivalent to about 200 mg of aurothioglucose, to a accurately weighed, to a 10-mL volumetric flask, dilute withbeaker containing 400 mL of acetone. W ash the pipet into the acetone to volume, and mix.beaker with a small quantity of acetone, mix, allow the solids to Chromatographic system (see Chromatography ⟨621⟩)—Thesettle, and decant the supernatant through a filter. W ash the gas chromatograph is equipped with a flame-ionization detectorsolids with another 400-mL portion of acetone, and repeat the and a 0.32-mm × 25-m fused silica capillar y column coateddecantation. Transfer the solids to the filter with the aid of ace- with phase G1. The column temperature is maintained at about

Official from May 1, 2012Copyright (c) 2011 The United States Pharmacopeial Convention. All rights reserved.

Accessed from 128.83.63.20 by nEwp0rt1 on Mon Nov 21 22:45:44 EST 2011