气相色谱-质谱联用法测定琥珀酸美托洛尔片中环氧氯丙烷的含量  

Determination of epichlorohydrin in Metoprolol Succinate Tablets by gas chromatography-mass spectrometry

作　　者：段澜波 梁春燕 黄丽丽 DUAN Lan-Bo;LIANG Chun-Yan;HUANG Li-Li(Sinopharm Zhijun(Shenzhen)Pharmaceutical Co.,Ltd.,Shenzhen 518000,China;Guilin Medical University,Guilin 541000,China;Guangxi Zhuang Autonomous Region Institute for Drug Control,Nanning 530001,China)

机构地区：[1]国药集团致君(深圳)制药有限公司,深圳518000 [2]桂林医学院药学院,桂林541000 [3]广西壮族自治区药品检验研究院,南宁530001

出　　处：《实验室检测》2024年第12期1-5,共5页Laboratory Testing

摘　　要：目的 建立气–质联用法测定琥珀酸美托洛尔片中环氧氯丙烷的含量。方法 色谱柱为HP-1MS;进样口温度为220℃;进样方式为分流进样,分流比为10∶1;升温程序为初始温度50℃保持3 min,再以20℃/min的速率升温至80℃并保持5 min,最后以40℃/min的速率升温至280℃并保持8 min;进样量为1μL。离子源为电子轰击源(EI),离子源温度为230℃;质谱传输接口温度为260℃;质谱监测模式为选择离子扫描(SIM);检测特征离子质荷比(m/z)为49、57、62。结果 环氧氯丙烷检测的质量浓度线性范围为30~120 ng/mL(r>0.99);检测限为32.37 ng/mL;定量限为107.89 ng/mL;进样精密度RSD为1.8%(n=6);准确度为103.8%,RSD为2.5%(n=6)。3批琥珀酸美托洛尔片,均未检出环氧氯丙烷。结论 建立的气–质联用法简便实用、准确可靠,适用于测定琥珀酸美托洛尔片中环氧氯丙烷的含量。Objective To establish a gas-mass spectrometry method for determination of epichlorohydrin in Metoprolol succinate tablets.Methods The chromatographic column is HP-1MS.Injection temperature is 220℃;The injection method is split injection,and the split ratio is 10∶1.The heating procedure is to keep the initial temperature at 50℃for 3 min,then raise the temperature to 80℃at a rate of 20℃/min for 5 min,and to 280℃at a rate of 40℃/min for 8 min.The sample intake capacity is 1μL.The ion source is electron bombardment source(EI),ion source temperature is 230℃.Mass spectrometry interface temperature is 260℃;the monitoring mode of mass spectrometry is SIM.The mass to charge ratios(m/z)are 49,57 and 62.Results The linear range of epichlorohydrin concentration is 30~120 ng/mL(r>0.99).The detection limit is 32.37 ng/mL.The limit of quantitation is 107.89 ng/mL.RSD of precision is 1.8%(n=6).The average recovery is 103.8%with RSD of 2.5%(n=6).Epichlorohydrin was not detected in 3 batches of Metoprolol succinate tablets.Conclusion The established gas-mass coupling method is simple,practical,accurate and reliable,and can be used for the determination of epichlorohydrin in Metoprolol succinate tablets.

关 键 词：气–质联用法 美托洛尔 环氧氯丙烷 

分 类 号：O657.63[理学—分析化学] TQ460.72[理学—化学]