顶空GC-FID法测定盐酸氯胺酮中的苯和4-甲基-3-戊烯-2-酮的残留量  

Determination of benzene and mesityl oxide residues in the ketamine hydrochloride by Headspace

作　　者：晏海军 陈一波 张福利[2] 林丽娅 YAN Haijun;CHEN Yibo;LIN Liya;ZHANG Fuli(College of Chemistry and Chemical Engineering,Shanghai University of Engineering Science,Shanghai 201620,China;Shanghai Institute of Pharmaceutical Industry,China State Institute of Pharmaceutical Industry,Shanghai 201203,China)

机构地区：[1]上海工程技术大学化学化工学院,上海201620 [2]中国医药工业研究总院上海医药工业研究院,上海201203

出　　处：《沈阳药科大学学报》2023年第10期1337-1341,1365,共6页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立顶空GC-FID法测定盐酸氯胺酮中的基因毒性杂质苯和4-甲基-3-戊烯-2-酮的残留量。方法采用Agilent DB-624毛细管柱(30 m×0.53 mm,3μm)和氢火焰离子化检测器,检测器温度250℃,进样口温度150℃,载气为氮气,顶空进样,分流比为5:1,平衡温度为95℃,平衡时间为25 min。结果苯和4-甲基-3-戊烯-2-酮在各自的质量浓度内呈良好的线性(r>0.9997),定量限分别为0.021和0.163 mg·L^(-1),平均回收率分别为93.6%和97.9%,RSD分别为3.2%和2.7%。结论该方法适用于盐酸氯胺酮中苯和4-甲基-3-戊烯-2-酮的检测。Objective To establish a headspace GC-FID method for the determination of genotoxic impurities benzene and mesityl oxide residues in ketamine hydrochloride.Methods The Agilent DB-624 capillary column and hydrogen flame ionization detector were used,the detector temperature was 250℃and the injection port temperature was 150℃.The carrier gas is nitrogen,headspace injection was used with the split ratio of 5∶1.The equilibrium temperature and time were set at 95℃and 25 min.Results Benzene and mesityl oxide show a good linear relationship in the self-concentration range(r>0.9997),and the limits of quantification were 0.021 and 0.163 mg·L^(-1).The average recovery rate were 93.6%and 97.9%while RSDs was 3.2%and 2.7%,respectively.Conclusion This method has high sensitivity,strong specificity and good accuracy,which is suitable for the detection of benzene and mesityl oxide in ketamine hydrochloride.

关 键 词：盐酸氯胺酮 基因毒性杂质 苯 4-甲基-3-戊烯-2-酮 顶空气相色谱 

分 类 号：R917[医药卫生—药物分析学]