明胶空心胶囊中有机溶剂残留量的分析方法研究

目的: 建立顶空进样-气相色谱-质谱联用法(HS-GC-MS)初筛定性、顶空进样-气相色谱-氢火焰离子化检测器(HS-GC-FID)定量测定药用明胶空心胶囊中有机溶剂残留量的检测方法。 方法: 采用HS-GC-MS,Scan模式定性鉴别残留溶剂的种类。采用HS-GC-FID检测器,定量测定明胶空心胶囊中丙酮、乙醇、三氯甲烷和甲苯4种有机溶剂的残留量。 结果: 在选定的色谱条件下,4种有机溶剂达到了完全分离,在所考察范围内线性关系良好,样品中的有机溶剂残留量均在规定限度范围内。 结论: 该法快速,准确,专属性强,可用于明胶空心胶囊中有机溶剂残留量的控制。

Objective: To establish HS-GC-MS and HS-GC-FID methods for determination of the residual organic solvents in vacant gelatin capsules. Method: HS-GC-MS Qualitative and screening mode was carried out.The 4 residual organic solvents including acetone,ethanol trichloromethane and toluene were determined by HS-GC-FIDinstrument coupled with headspace sampler in vacant gelatin capsules. Result: At the selected chromatographic conditions,4 kinds of residual organic solvents could get completely separation.The linear regression coefficients between peak areas and concentration were good.The contents of 4 kinds of residual organic solvents in sample were all in the limit range of define. Conclusion: This method is rapid,accurate,selective and suitable for determine the residual organic solvents in vacant gelatin capsules.

1 ChP(中国药典).2010.Vol Ⅱ(二部):Appendix(附录)ⅧP
2 ZHOU Hai-jun(周海钧).Drug Registration Intrenational Technical Requirements(药品注册的国际技术要求).Beijing(北京):People's Medical Publishing House(人民卫生出版社),2000.87
3 ZHU Xiao-hong(朱小红),LI Tao(李涛),ZHU Jian-rong(朱建荣).Identification of benzodiazepine drugs by GC-MS(苯二氮卓类药物的气相色谱-质谱联用法定性分析方法研究).Chin J Pharm Anal(药物分析杂志),2011,32(12):2289
4 LI Tao(李涛),ZHU Xiao-hong(朱小红), LIN Fang(林芳).GC-MS determination of chemical drugs added illegally in chinese patent medicine and health food(GC-MS联用方法检测降压类中成药及保健食品中非法添加的化学药物). Chin J Pharm Anal(药物分析杂志),2010,31(12):2212
5 WU Chun-li (吴春丽),QIAO Jia-bin(乔家彬),LEI Wei(雷伟).Determination of residual organic solvents in levofloxacin mesylate by gas chromatography(甲磺酸左氧氟沙星中有机溶剂残留量的气相色谱法测定).J Zhengzhou Univ (Med Sci),2012(2):254
6 SHEN Shu-chang(申书昌),YUN Dan(云丹),LI Fei(李飞).Determination of dichloromethane and trichloromethane residues in ranitidine hydrochloride by headspace liquid phase microextraction coupled with gas chromatography(顶空液相微萃取-气相色谱法测定盐酸雷尼替丁中二氯甲烷和三氯甲烷的残留量).Chin J Chromatogr (色谱),2009(6):845
7 NING Wei-zhi(宁伟志),WU Xiu-rong(吴秀荣),LIN Huan-ze(林焕泽).Determination of residual solvents in valaciclovir hydrochloride by headspace gas chromatography(顶空气相色谱法测定盐酸伐昔洛韦中的残留溶剂).China Pharm(中国药房),2012(9):832
8 ZHANG Zai-juan(张在娟),LU Di(逯荻),CUI Li-xia(崔丽霞),et al.Determination of residual solvents in Naomaitong soft capsule by headspace GC(顶空进样气相色谱法测定脑脉通软胶囊中有机溶剂残留量).Tianjin J Tradit Chin Med(天津中医药),2011,28(6):506
9 WEI Ning-yi(魏宁漪),WU Jian-min(吴建敏),ZHANG Qi-ming(张启明).GC-MS determination of related substance in alltride and study on its stability(GC-MS法测定大蒜素有关物质和稳定性研究).Chin J Pharm Anal(药物分析杂志),2011,31(9):1699
10 FAN Ming-wei(樊敏伟),QING Jing(秦晶),HE Hong-wei(何红伟),et al.Determination of organic residues from macroporous adsorption resin in St.John’s Wort extract by capillary gas chromatography with headspace sampling(顶空气相色谱法测定贯叶金丝桃提取物中大孔树脂有机溶剂残留).Chin Tradit Pat Med(中成药),2011,33(10):1748
11 WANG Yong-hua(王永华).Theory and technology of headspace gas chromatograph analysis(顶空气相色谱分析原理与技术). Environ Monit China(中国环境监测),2006,22(2):7
12 FU Qiang(傅强).Traditional Chinese Drug Analysis(中药分析).Beijing(北京):Chemical Industry Publishing Company(化学工业出版社),2010.31