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目的建立测定佐芬普利钙中间体(S)-(?)-3-苯甲酰巯基-2-甲基丙酸的光学异构体杂质(R)-(+)-3-苯甲酰巯基-2-甲基丙酸含量的柱前衍生化GC。方法以高纯试剂D-(+)-2-辛醇对(S)-(?)-3-苯甲酰巯基-2-甲基丙酸样品进行衍生化处理,衍生产物以Agilent DB-1701(30 m×0.53 mm,1.0μm)柱为分析柱,以氮气为载气,流速为2.0 m L·min?1,检测器温度为250℃,进样口温度为200℃,柱温为程序升温,进样量为1.0μL。结果光学杂质(R)-(+)-3-苯甲酰巯基-2-甲基丙酸在3.22~121.44μg·m L?1内线性关系良好(r=0.995 2),定量限为3.22μg·m L?1,加样回收率为99.6%~102.4%,日内和日间精密度RSD均<2.0%。结论该方法操作简便、专属性强,试剂成本低廉、易得,结果准确性高、重复性好,可用于佐芬普利钙中间体(S)-(?)-3-苯甲酰巯基-2-甲基丙酸光学杂质的含量测定。
OBJECTIVE To establish a method for the determination of optical isomers of (Z) - (+) - 3-benzoyl Pre-column Derivatization of Mercapto-2-methyl Propionic Acid. Methods The derivatization of (S) - (?) - 3 - benzoylmercapto - 2 - methyl propionic acid with D - (+ (30 m × 0.53 mm, 1.0 μm) column was used as the analytical column. Nitrogen gas was used as the carrier gas at a flow rate of 2.0 m L · min -1. The detector temperature was 250 ℃ and the inlet temperature was 200 ℃. Heating, injection volume of 1.0μL. Results There was a good linearity (r = 0.995 2) for optical impurity (R) - (+) - 3-benzoylmercapto-2-methylpropionic acid in the range of 3.22 ~ 121.44 μg · m L · 1, · M L · 1, the recoveries of samples were 99.6% ~ 102.4%, RSD of intra-day and inter-day precision were both less than 2.0%. Conclusion The method is simple and convenient, the specificity is high, the reagent cost is low, the result is easy to obtain, the result is accurate and the repeatability is good. The method can be used for the determination of zofenopril calcium intermediate (S) - (?) - Determination of 2-methylpropionic acid optical impurities.