天然冰片、艾片、合成冰片中残留溶剂测定及风险分析  

Determination and risk analysis of residual solvents in Borneolum,L-Borneolum and Borneolum Syntheticum

作　　者：沈敏[1] 黄逸文 鲁辉 郭青 闵春艳 SHEN Min;HUANG Yi-wen;LU Hui;GUO Qing;MIN Chun-yan(Suzhou Vocational Health College,Suzhou 215000,China;Suzhou Institute for Drug Control,Suzhou 215000,China;Jiangsu Institute for Food and Drug Control,Nanjing 210019,China)

机构地区：[1]苏州卫生职业技术学院,江苏苏州215000 [2]苏州市药品检验检测研究中心,江苏苏州215000 [3]江苏省食品药品监督检验研究院,江苏南京210019

出　　处：《中成药》2023年第6期1914-1920,共7页Chinese Traditional Patent Medicine

基　　金：国家药典委员会药品标准制修订研究课题(2018Z046)。

摘　　要：目的对天然冰片、艾片、合成冰片纯化工艺中正庚烷、正己烷、环己烷、异辛烷、乙酸乙酯、乙醇残留量进行控制。方法建立顶空气相色谱法,DB-624毛细管柱(30 m×0.53 mm,3.0μm);FID检测器;程序升温。对34批天然冰片、12批艾片、34批合成冰片测定残留溶剂,并进行风险分析。结果天然冰片中部分批次检出乙醇,部分批次同时检出正己烷、环己烷、异辛烷和正庚烷,44%样品正己烷超标;艾片中部分批次检出正己烷、环己烷和异辛烷,残留量均符合规定;合成冰片中所有批次均同时检出正己烷、环己烷、异辛烷、正庚烷,残留量均符合规定。结论3种冰片中有机溶剂均有不同程度的残留,且残留量与其纯度有一定的关系。其中天然冰片中正己烷的残留带来的风险较高,建议在其质量标准中增加对正己烷的控制。AIM To determine and control the residuals of ethanol,n-hexane,ethyl acetate,cyclohexane,isooctane and n-heptane in Borneolum,L-Borneolum and Borneolum Syntheticum.METHODS The established method of headspace gas chromatography with a FID detector using DB-624(30 m×0.53 mm,3.0μm)as the capillary column through programmed temperature rise was applied upon thirty-four batches of Borneolum,twelve batches of L-Borneolum,and thirty-four batches of Borneolum Syntheticum for the risk analysis.RESULTS Borneolum was observed with ethanol in some batches;and concomitant n-hexane,cyclohexane,isooctane,n-heptane in some batches;and totally 44%n-hexane exceeding the specifications.L-Borneolum was detected with n-Hexane,cyclohexane and isooctane in some batches,and yet the residual amounts were all within the specifications limits.All batches of Borneolum Syntheticum were detected with residual n-hexane,cyclohexane,isooctane and n-heptane within the specifications limits.CONCLUSION Because three kinds of borneol are generally found with residual solvents whose quantity are proportionally associated with the purity,in particular,the residual n-hexane-generated high risk in Borneolum,we suggest to include the control of n-hexane into the quality specification of Borneolum.

关 键 词：天然冰片 艾片 合成冰片 残留溶剂 顶空气相色谱 风险分析 

分 类 号：R283[医药卫生—中药学]