LLE-GC-MS法同时测定甘磷酸胆碱中的缩水甘油和3-氯-1,2-丙二醇  被引量:1

Simultaneous determination of glycidol and 3-monochloro-1,2-propanediol in L-α-glycerophosphorylcholine by LLE-GC-MS

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作  者:王鑫[1] 崔烨帆 于治国[1] 于淼[1] 赵云丽[1] WANG Xin;CUI Yefan;YU Zhiguo;YU Miao;ZHAO Yunli(School of Pharmacy,Shenyang Pharmaceutical University,Shenyang 110016,China)

机构地区:[1]沈阳药科大学药学院,辽宁沈阳110016

出  处:《沈阳药科大学学报》2023年第8期1011-1019,共9页Journal of Shenyang Pharmaceutical University

基  金:辽宁省百千万人才工程资助项目(2111520241)。

摘  要:目的 建立液液萃取-气相色谱-质谱法(LLE-GC-MS)同时测定甘磷酸胆碱原料药中的基因毒性杂质缩水甘油和3-氯-1,2-丙二醇。方法 采用酸性氯化钠溶液和酸性无水硫酸钠溶液分别处理甘磷酸胆碱原料药,经硅藻土柱净化、富集后用七氟丁酰基咪唑衍生,采用气相色谱-质谱法(SIM模式)进行检测,以D5-3-氯-1,2丙二醇作为内标,通过双样本差减法计算样品中缩水甘油和3-氯-1,2-丙二醇的含量。结果 2种基因毒性杂质与内标物的峰面积比值在0.1~2 mg·L^(-1)浓度范围内呈线性相关,相关系数(r)均不小于0.999 2,样品的加样回收率为86.4%~103.3%(RSD<6.0%,n=9)。结论 该方法灵敏度高、专属性强,适用于甘磷酸胆碱原料药中缩水甘油和3-氯-1,2-丙二醇的测定。Objective To establish a method for simultaneous determination of genotoxic impurities including glycidol and 3-monochloro-1,2-propanediol in L-α-glycerophosphorylcholine through liquid-liquid extraction(LLE)coupled with gas chromatography-mass spectrometry(GC-MS).Methods The samples were treated with acid sodium chloride solution and acid anhydrous sodium sulfate solution respectively,and them purified using diatomite extraction columns.The target analytes in extraction solution were derived with heptafluorobutyrylimidazole,then the derivatives were determined by gas chromatography-mass spectrometry(SIM mode)with D_5-3-monochloro-1,2-propanediol as internal standard.The contents of glycidol and 3-monochloro-1,2-propanediol in L-α-glycerophosphorylcholine were calculated by two-sample subtraction method.Results The calibration curves showed good linear relationships(r≥0.9992)within the concentration range of 0.1-2 mg·L^(-1).The recoveries ranged from 86.4%to 103.3%(RSD6.0%,n=9).Conclusion The method has the advantages of good sensitivity and specificity,and can be used for the determination of glycidol and 3-monochloro-1,2-propanediol in L-α-glycerophosphorylcholine.

关 键 词:LLE-GC-MS法 甘磷酸胆碱 基因毒性杂质 缩水甘油 3-氯-1 2-丙二醇 

分 类 号:R917[医药卫生—药物分析学]

 

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