摘要
建立高效液相色谱法测定六神曲中乳酸对映异构体的含量,并对样品提取方法进行优化.样品经粉碎后,用纯化水超声提取,10 000 r/min离心5min.上清液经滤膜过滤后,以2 mmol/L CuSO_(4)溶液(5%的异丙醇溶液为溶剂)为流动相,设定流速为0.60 mL/min洗脱,经Chirex 3126 (D)-penicillami(4.6 mm×250 mm,5μm)色谱柱进行手性拆分,二极管阵列检测器测定,外标法定量.结果表明,L-乳酸、D-乳酸在各自范围内线性关系良好(r≥0.999 7),平均加样回收率分别为98.5%、97.1%,相对标准偏差(RSD)分别为1.8%和2.4%.方法简便可行,稳定可靠,可为六神曲的品质提升提供参考.
The method for the determination of lactic acid enantiomers in Massa Medicata Fermentata by high performance liquid chromatography(HPLC)was established,and the sample extraction method was optimized.The sample was crushed and extracted using ultrasonic extraction with purified water,centrifuged at 10000 r/min for 5 min.The supernatant was filtered using a filter membrane,eluted with 2 mmol/L CuSO4 solution(5%isopropyl alcohol as solvent)as mobile phase at a flow rate of 0.60 mL/min,separated chirally on a Chirex 3126(D)-penicillami(4.6 mm×250 mm,5μm)column,and detected using a diode array detector,quantified by external standard method.The results showed that L-lactic acid and D-lactic acid had good linearities in their ranges(r≥0.9997),and the average recoveries were 98.5%and 97.1%,respectively.The relative standard deviations(RSD)were 1.8%and 2.4%,respectively.The method is simple,feasible,stable,and reliable,and can provide a reference for the quality improvement of Massa Medicata Fermentata.
作者
李运
杜锐浒
张晓萍
韩晓霞
王月玲
许晓辉
戚鹏飞
LI Yun;DU Ruihu;ZHANG Xiaoping;HAN Xiaoxia;WANG Yueling;XU Xiaohui;QI Pengfei(Lanzhou Institute for Food and Drug Control,Lanzhou 730050,China;School of Pharmacy,Lanzhou University,Lanzhou 730000,China)
出处
《分析测试技术与仪器》
CAS
2024年第6期360-365,共6页
Analysis and Testing Technology and Instruments
基金
陇原青年创新创业人才项目(2023LQGR49)
甘肃省药品科研项目(2022GSMPA0037)
兰州市青年科技人才创新项目(2023-QN-144)。