摘要
目的:利用柱前衍生-反相高效液相色谱法,完善在合成盐酸伪麻黄碱生产过程中的杂质的限度检查,为生产过程的杂质控制提供依据。方法:以(1S)-(+)-氯甲酸薄荷醇酯作为手性衍生化试剂,采用Phenomenex Luna C18柱(250mm×4.6mm,5μm),以乙腈-水-醋酸-三乙胺(29∶20∶0.2∶0.01)为流动相,流速1.0mL·min-1,在254nm处检测。结果:盐酸伪麻黄碱、盐酸左伪麻黄碱、盐酸右麻黄碱、盐酸麻黄碱的浓度均在0.033～0.667μg·mL-1范围内线性关系良好(r>0.99);检测限(S/N=3)分别为56,56,58,56ng;定量限(S/N=10)分别为210,204,226,216ng;各对映体均达到基线分离。结论:方法快速、简便,重复性好,灵敏度高,可用于对合成盐酸伪麻黄碱生产过程中产生的光学异构体进行控制。
Objective： To establish an RP - HPLC with pre - column derivatization method for determination of im- purities in synthetic pseudoephedrine hydrochloride, to set up limits of impurities for pseudoephedrine hydrochloride in production process. Methods： （ 1S ） - （ ＋ ） - menthyl chloroformate was used as chiral derivatization rea- gent. The separation was carried out on a Phenomenex Luna C18 column（250 mm ×4.6 mm,5 μm） with a mixture of acetonitrile - water - acetic acid - triethylamine（29： 20： 0. 2： 0. 01 ） as the mobile phase pumped at a flow rate of 1.0 mL ·min - 1, and the detection wavelength was 254 nm. Results： The calibration curves of （ ＋ ） - pseudoephed- fine hydrochloride, （ - ） - pseudoephedrine hydrochloride, （ ＋ ） - ephedrine hydrochloride, and （ - ） - ephedrine hydrochloride were linear in the range of 0. 033 - 0. 667 μg · mL - 1 （ r 〉 0. 99） ; The detection limits （ S/N = 3） were 56,56,58,56 ng respectively; The quantitation limits （ S/N = 10 ） were 210,204,226,216 ng respectively; each of optical isomers was well isolated. Conclusion： The method is sensitive, accurate and suitable for optical isomer con- trol in the manufacturing of synthetic pseudoephedrine hydrochloride.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第9期1504-1506,共3页
Chinese Journal of Pharmaceutical Analysis
