蛋黄卵磷脂在中国药典标准中残留溶剂测定方法的优化  

Optimization of Residual Solvent Determination of Egg Yolk Lecithin in Chinese Pharmacopoeia

作　　者：魏嘉利 赵恂 陈蕾[4] 张玫 袁耀佐 柳文媛[1] WEI Jiali;ZHAO Xun;CHEN Lei;ZHANG Mei;YUAN Yaozuo;LIU Wenyuan(Department of Pharmaceutical Analysis,China Pharmaceutical University,Nanjing 210009,China;Jiangsu Institute For Food and Drug Control,Nanjing 210019,China;NMPA Key Laboratory for Impurity Profile of Chemical Drugs,Nanjing 210019,China;Chinese Pharmacopoeia Commission,Beijing 100061,China)

机构地区：[1]中国药科大学药物分析系,南京210009 [2]江苏省食品药品监督检验研究院,南京210019 [3]国家药品监督管理局化学药品杂质谱研究重点实验室,南京210009 [4]国家药典委员会,北京100061

出　　处：《中国现代应用药学》2023年第8期1091-1095,共5页Chinese Journal of Modern Applied Pharmacy

基　　金：国家药典委员会药品标准制修订(2020Y002);江苏省药品监督管理局科研计划课题(24)。

摘　　要：目的建立顶空气相色谱法测定蛋黄卵磷脂中的石油醚、乙醇、乙醚、丙酮、正己烷共5种残留溶剂的含量,并采用气相色谱-质谱联用技术,结合质谱数据检索对样品中的其他挥发性杂质进行结构鉴定。方法GC条件为色谱柱:DB-624UI毛细管柱(60 m×0.25 mm,1.4μm),采用程序升温;检测器:氢火焰离子化检测器;检测器温度:250℃;分流比:20∶1。GC-MS条件为GC条件的载气:氦气、不分流模式进样,其余条件同上述GC条件。质谱条件的离子源温度:230℃;接口温度:230℃;采用电子轰击离子源;电离能量:70 eV;扫描方式:Q3Scan;扫描范围:m/z 45~500;检测时间:7~28.5 min。结果5种溶剂的分离度良好,样品中其他挥发性杂质对5种待测组分的检测无影响;5种成分在各自浓度范围内呈良好的线性关系(r>0.999);检测限范围为(0.003~0.13)μg·mL^(–1),定量限范围为(0.017~0.21)μg·mL^(–1);平均回收率为93.74%~104.31%;精密度、重复性的RSD均<5%。结论本方法操作简便、灵敏度高,可以用于测定蛋黄卵磷脂中的残留溶剂。OBJECTIVE To establish a headspace gas chromatography method for the determination of five kinds of residual solvents in egg yolk lecithin,such as petroleum ether,ethanol,diethyl ether,acetone and n-hexane.Using gas chromatography-mass spectrometry technology,the mass spectrometry retrieval data for other volatile impurities in the sample were combined to identify the structure.METHODS GC conditions were column:DB-624UI capillary column(60 m×0.25 mmm 1.4μm),the column temperature was raised by program;Detector:flame ionization detector;detector temperature:250℃;Split ratio:20∶1.GC-MS conditions were GC conditions:the carrier gas was helium,the remaining conditions accorded with GC conditions above.MS conditions were ion source temperature:230℃;the interface temperature was set at 230℃;using electron impact inoization;EI energy:70 eV;scanning mode:Q3Scan mode;scan range:m/z 45−500;detection time:7.00−28.50 min.RESULTS The 5 residual solvents tested were completely separated,other volatile impurities in the sample had no influence on the 5 residual solvents.The linear relationship was good in the concentration range(r>0.999);limit of detection were(0.003−0.13)μg·mL^(-1),limit of quantitation were(0.017−0.21)μg·mL^(-1);average recoveries were 93.74%−104.31%;accuracy and repeatability were<5%.CONCLUSION The method is simple,highly sensitive and reproducible,it can be used to determine the residual solvents in egg yolk lecithin.

关 键 词：蛋黄卵磷脂 残留溶剂 顶空气相色谱法 

分 类 号：R917.101[医药卫生—药物分析学]