GC-MS法测定甘磷酸胆碱中环氧氯丙烷和缩水甘油的含量  

Determination of epichlorhydrin and glycidol in choline glycerophosphate by GC-MS

作　　者：王倩 王雪芹[1] 朱艳春 吕海鸿[1] 张竞[1] WANG Qian;WANG Xue-qin;ZHU Yan-chun;LU Hai-hong;ZHANG Jing(Henan Provincial Institute for Food and Drug Control,Zhengzhou 450008,China)

机构地区：[1]河南省食品药品检验所,郑州450008

出　　处：《药物分析杂志》2023年第4期630-635,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：河南省市场监督管理局科技计划项目(2020sj27)。

摘　　要：目的:建立气相色谱-质谱联用法测定甘磷酸胆碱中环氧氯丙烷和缩水甘油2个毒性杂质的含量。方法:样品用甲醇溶解并稀释,采用ZB-WAXplusTM(30 m×0.25 mm, 0.25μm)色谱柱,柱温为程序升温(初始温度30℃,保持1 min,以30℃·min^(-1)的速率升温至220℃,保持5 min),进样口温度为200℃,不分流进样,载气为高纯氦气(He),进样口为恒流模式,进样量为1μL;离子源为电子轰击源(EI),电离电压70 eV,离子源温度200℃,质谱传输接口温度250℃,质谱监测模式为选择离子监测(SIM),环氧氯丙烷检测离子质荷比为49、57、62,缩水甘油检测离子质荷比为31、43、44。溶剂延迟为3 min。按外标法定量。结果:环氧氯丙烷质量浓度在29.86~746.48 ng·mL^(-1)范围内,线性良好,相关系数为0.999 7;检测限为19.91 ng·mL^(-1),定量限为29.86 ng·mL^(-1);仪器的精密度和方法的重复性RSD均<10%;平均回收率(n=9)为93.9%,RSD为5.1%。缩水甘油质量浓度在172.91~922.18 ng·mL^(-1)范围内,线性良好,相关系数为0.999 4;检测限为115.27 ng·mL^(-1),定量限为172.91 ng·mL^(-1);仪器的精密度和方法的重复性RSD均<10%;平均回收率(n=9)为91.4%,RSD为3.1%。4批样品中,环氧氯丙烷和缩水甘油2个杂质均未检出。结论:该方法简单高效,重复性好,可用于检测甘磷酸胆碱中环氧氯丙烷和缩水甘油2个毒性杂质的含量。Objective:To establish a method for determination of two tomix impurities(epichlorhydrin and glycidol)in choline glycerophosphate by GC-MS.Methods:Sample was dissolved and diluted with methanol.The determination was performed on ZB-WAXplus~(TM)column(30 m×0.25 mm,0.25μm),the column temperature was programmed temperature(initially heated at 30℃for 1 min,rose to 220℃at a speed of 30℃·min^(-1)remaining 5 min).using high purity He as carrier gas,the injector temperature was 200℃,splitless,the sample volume was 1μL,The ion source was electrospray ion source,the ion source temperature was 200℃,the ionization energy was 70 eV,Transmission line temperature was 250℃,the scan mode was selective ion monitoring(SIM),the ion mass charge ratio(m/z)of epichlorhydrin were 49,57,62,the m/z of glycidol were 31,43,44,the solvent delay was 3 min,qualitified by the external reference method.Results:Epichlorhydrin showed a good linear relationship(r=0.9997)in the concentration range of 29.86-746.48 ng·mL^(-1),the LOD was 19.91 ng·mL^(-1),the LOQ was 29.86 ng·mL^(-1),RSDs of precision and repeatability were less than 10%.The average recovery(n=9)was 93.9%with RSD of 5.1%.Glycidol showed a good linear relationship(r=0.9994)in the concentration range of 172.91-922.18 ng·mL^(-1),LOD was 115.27 ng·mL^(-1),the LOQ was 172.91 ng·mL^(-1),RSDs of precision and repeatability were less than 10%.The average recovery(n=9)was 91.4%with RSD of 3.1%.In the 4 batches of samples tested,the contents of epichlorhydrin and glycidol were negtive.Conclusion:This method is simple,efficient and repeatable,it can be used to determine the contents of epichlorhydrin and glycidol in L-α-glycerophosphorylcholine.

关 键 词：气相色谱-质谱联用法 环氧氯丙烷 缩水甘油 甘磷酸胆碱 选择离子监测 外标法 

分 类 号：R917[医药卫生—药物分析学]