GC-MS手性拆分活血止痛制剂冰片成分及含量测定  

Chiral Separation and Content Determination of Borneol in Huoxue Zhitong Preparations by GC-MS

作　　者：曹玉 史达 陈洁 张玲[1,2] Cao Yu;Shi Da;Chen Jie;Zhang Ling(Nanjing Institute for Food and Drug Control,Nanjing 21112,China;College of Pharmacy,Nanjing Medical University)

机构地区：[1]南京市食品药品监督检验院,南京211112 [2]南京医科大学药学院

出　　处：《中国药师》2022年第9期1677-1681,共5页China Pharmacist

基　　金：江苏省市场监督管理局2020年度科技计划项目(编号:KJ207564)。

摘　　要：目的:应用气相色谱质谱(GC-MS)法建立同时测定活血止痛胶囊、活血止痛片、活血止痛软胶囊中左旋樟脑、右旋樟脑、左旋龙脑、右旋龙脑及异龙脑对映异构体检测方法,并建议制剂中成分限度要求。方法:采用GC-MS法,以手性毛细管色谱柱分离测定,采用选择离子检测(SIM)模式选择m/z 95为左旋樟脑、右旋樟脑、左旋龙脑、右旋龙脑、异龙脑检测离子,选择m/z 128为内标萘检测离子,通过内标法同时对活血止痛制剂中5个主要挥发性成分进行定量分析。结果:活血止痛胶囊、片、软胶囊中左旋龙脑、右旋龙脑、左旋樟脑、右旋樟脑及异龙脑在20min内全部检出,分离度良好,在各自的浓度范围内均有良好的线性关系(r≥0.9993);平均回收率在95.1%~107.4%范围内,RSD为1.2%~7.5%(n=6)。结论:经方法学验证,该方法简便、灵敏、准确,可用于活血止痛片、胶囊及软胶囊中龙脑、异龙脑、樟脑的检测,为其质量评估及风险监控提供技术参考。Objective:To establish a method for the simultaneous determination of L-camphor,D-camphor,levorotatory borneol,dextral borneol and isoborneol enantiomers in Huoxue Zhitong capsules,Huoxue Zhitong tablets and Huoxue Zhitong soft capsules by GC-MS,and to suggest the composition limit requirements for the preparations.Methods:GC-MS was used by chiral capillary chromatographic column separation with detection ion m/z 95 for L-camphor,D-camphor,levorotatory borneol,dextral borneol and isoborneol,and m/z 128 for the internal standard naphthalene.The five main active components in Huoxue Zhitong preparations were quantitatively analyzed by the internal standard method.Results:L-Camphor,D-camphor,levorotatory borneol,dextral borneol and isoborneol in Huoxue Zhitong capsules,tablets and soft capsules were all detected within 20 min with good separation degree and good linear relationship within their concentration ranges(r≥0.9993).The average recoveries were between 95.1%and 107.7%with the RSDs of 1.2%-7.5%.Conclusion:The method is simple,sensitive and accurate,and can be used for the detection of borneol,isoborneol and camphor in Huoxue Zhitong tablets,capsules and soft capsules,which provides technical reference for the quality assessment and risk monitoring.

关 键 词：气相色谱质谱法 活血止痛 樟脑 龙脑 手性柱 

分 类 号：R927.2[医药卫生—药学]