普罗布考USP翻译.docx

普罗布考Phenol,4,4‘-[(1-methylethylidene)bis(thio)]bis[2,6-bis(1,1-dimethylethyl)Acetone bis(3,5-di-tert-butyl-4-hydroxyphenyl) mercaptole [23288-49-5].4,4’ -[(1-甲基亚乙基)二硫]双[2,6-二(1,1-二甲乙基)苯酚]双 (3， 5-二叔丁基羟基苯硫)缩丙酮Probucol contains not less than 98.0 percent and not more than 102.0 percent of C H O S , calculated on the dried basis.31 48 2 2按干燥品计算，普罗布考含C31H48O2S2应为98.0%〜102.0%31 48 2 2Packaging and storage- Preserve in well-closed , light-resistant containers.包装与贮存：密封，遮光保存USP REFERENCE STANDARDS <11 > 美国药典标准品USP Probucol RS 美国药典普罗布考对照品USP Probucol Related Compound A RS2,2',6,6'-Tetra-tert-butyldiphenoquinone.CHO28 40408.63美国药典普罗布考有关化合物A对照品2,2',6,6'-四叔丁基二苯醌USP Probucol Related Compound B RS 4,4'-(Dithio)bis(2,6-di-tert-butylphenol).C28H42O474.78美国药典普罗布考有关化合物B对照品4,4'-(二硫)双(2,6-二叔丁基苯酚)USP Probucol Related Compound C RS4-[(3,5-Di-tert-butyl-2-hydroxyphenylthio)isopropylidenethtio]-2,6-di-ter t-butylphenol.C31H4802S2 516.86美国药典普罗布考有关化合物C对照品4-［（3,5-二叔丁基-2-羟苯硫）亚异丙基硫］-2,6-二叔丁基苯酚Identification, Infrared Absorpti . 鉴别，红外吸收< 197K > 项下.MELTiNG RANGE, Class / < 741> : between 124°and 127°, a dried specimen being used.熔点范围，按Class / < 741>项下测定：干燥样品应为124°〜127°LOSS ON DRYING <731 >— Dry it in vacuum at 80° for 1 hour: it loses not more than l.0% of its weight.干燥失重，按＜731 ＞项下测定，80°减压干燥1小时，减失重量不得 过 1.0% 。

RESIDUE ON IGNITION <281 > : 0.1 %.炽灼残渣，按<281 >项下测定：0.1 %HEAVY METALS, Method //< 231 >: 0.002%.重金属，按< 231 >项下第II法：0.002%Related compounds— 有关化合物.Mobile phase—Prepare a mixture of n-hexane and dehydrated alcohol (4000:1). Make adjustments， if necessary (see Systerm Suitability under chromatography <621>) 流动相—正己烷和无水乙醇按 4000:1 配制如果有必要，可以适当 调整(见色谱法<621>项下)Reference solution 1 — Dissolve an accurately weighed quantity of USP Probucol Related Compound A RS in n-hexane， and dilute quantitatively and stepwise with n-hexane to obtain a solution having a known concentration of about 10 pg per mL.参比溶液1—将精密称定的USP普罗布考有关化合物A对照品溶解 于正己烷中，并用正己烷稀释至浓度约为10pg/mL。

Reference solution2-Dissolve an accurately weighed quantity of USP Probucol Related Compound B RS in n-hexane， and dilute quantitatively with n-hexane to obtain a solution having a known concentration of about 0.1 mg per mL.参比溶液2—将精密称定的USP普罗布考有关化合物B对照品溶解 于正己烷中，并用正己烷稀释至浓度约为 0.1mg/mLReference solution 3- Dissolve an accurately weighed quantity of USP Probucol Related Compound C RS in n-hexane, and dilute quantitatively with n-hexane to obtain a solution having a known concentration of about l mg per mL.参比溶液3—将精密称定的USP普罗布考有关化合物C对照品溶解 于正己烷中，并用正己烷稀释至浓度约为 1mg/mL。

Standard solution—Transfer about 10 mg of USP Probucol RS, accurately weighed, to a 50-mL volumetric flask. Add l mL of Reference solution 1, 4 mL of Reference solution 2, and 10 mL of Reference solution 3, and dilute with n- hexane to volume.标准溶液一精密称取约10mg美国药典普罗布考对照品，置50ml容 量瓶中加入1ml参比溶液1、4ml参比溶液2和10ml参比溶液3, 并加入正己烷稀释至刻度Test solution—Transfer about l g of Probucol, accurately weighed, to a 25-mL volumetric flask,dissolve in and dilute with n-hexane to volume, and mix.供试溶液一精密称取普罗布考约1g，置25ml容量瓶中，加入正己烷 稀释至刻度，混匀。

System suitability solution—Pipet 1ml of Reference solution 2 and 1ml of the Test solution into a 200-mL volumetric flask, dilute with n-hexane to volume, and mix.系统适应性溶液一吸取1ml参比溶液2和1ml供试溶液，置200ml 容量瓶中，加入正己烷稀释至刻度，混匀Chromatographic system (see CHROMATOGRAPHY <62 1>) —The liquid chromatograph is equipped with 254-nm and 420-nm detectors, connected in series, and a 4.6-mm x 25-cmcolumn that contains packing L3. The flow rate is about l mL per minute. Chromatograph theSystem suitability solution, and record the peak responses detected at254 nm, for related compound B and probucol. Related compound B elutes first, the resolution, R, of the peaks is not less than 2.5, and the relative standard deviation for replicate injections, determined from the probucol peak, is not more than 2%.色谱系统(见色谱法<621>项下)一配备254nm和420nm检测器及 填充L3(多孔硅胶微粒，即一般的硅胶柱)材质的4.6mmx 25cm色 谱柱的液相色谱仪。

流速约为1ml/分钟将系统适应性溶液注入色谱 仪，记录色谱峰，在254nm检测有关化合物B和普罗布考有关化 合物B先流出，峰的分离度R应不低于2.5，重复注射，普罗布考峰 面积的相对标准差应不大于2%Procedure—Separately inject equal volumes (about 20 /L) of theStandard solution and the Test solution into the chromatograph, record the chromatograms, and measure the peak areas. The order of elution is compound C, compound B, compound A, and finally probucol. Compound A is detected at 420 nm, and the others are detected at 254 nm. Calculate the percentage of each related compound in the portion of Probucol taken by the formula:2500(C / W)(r / r )usin which C is the concentration, in mg per mL, of the respectiveprobucol related compound in the Standard solution; W is the weight, in mg, of Probucol taken; and r and r are the peak areas obtained from the usTest solution; and the Standard solution, respectively: not more than 0 .0005% of compound A; not more than 0.02% of compound B; and not more than 0.5% of compound C are found.测定方法一将等体积(约。