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《化学分析计量》 2022年第05期
DOI:10.3969/j.issn.1008-6145.2022.05.006
高效液相色谱-质谱联用法同时测定盐酸二甲双胍肠溶片中6种亚硝胺类基因毒性杂质
徐艳梅,李挥,张素平,乔晓宁,苗会娟,盖成,王茉莉,高燕霞
河北省药品医疗器械检验研究院,石家庄 050200 
Simultaneous determination of 6 nitrosamine genotoxic impurities in metformin hydrochloride enteric-coated tablets by high performance liquid chromatography-mass spectrometry
徐艳梅,李挥,张素平,乔晓宁,苗会娟,盖成,王茉莉,高燕霞
Hebei Provincial Institute of Drug and Medical Device Inspection, Shijiazhuang 050200 
摘要:建立高效液相色谱-质谱联用法同时测定盐酸二甲双胍肠溶片中6种N-亚硝胺类基因毒性杂质(N-亚硝基二甲胺、N-亚硝基-N-甲基-4-氨基丁酸、N-亚硝基二乙胺、N-亚硝基乙基异丙胺、N-亚硝基二异丙胺和N-亚硝基二丁胺)。采用ACE C柱(150 mm×4.6 mm, 5μm),流动相为0.1%甲酸水-甲醇,流量为0.6 mL/min,梯度 18 洗脱,柱温为40℃,采用正离子多反应监测(MRM)模式,以大气压化学电离源为离子源。6种N-亚硝胺类基因毒性杂质的质量浓度在各自的线性范围内与色谱峰面积线性关系良好,相关系数均不小于0.999 5。检出限和定量限分别为0.033 7~0.0338 9 ng/mL和0.100 76~0.102 68 ng/mL。样品平均加标回收率为97.83%~103.33%,测定结果的相对标准偏差为1.19%~4.45%(n=9)。该方法专属性强,简单、快速、灵敏,适用于测定盐酸二甲双胍肠溶片中的N-亚硝胺类基因毒性杂质。 
Abstract:A high performance liquid chromatography-mass spectrometry method for the determination of 6 N-nitrosamine genotoxic impurities (N-nitrosodimethylamine, N-nitrosoethylisopropylamine, N-nitrosodiethylamine, N-nitroso-N-methyl-4-aminobutyric acid, N-nitrosodibutylamine, N-nitroso diisopropylamine) in metformin hydrochloride enteric-coated tablets simultaneously was established. The method was carried out on ACE C18 column (150 mm×4.6 mm, 5 18 μm). And mobile phase was 0.1% formic acid water(A)-methanol(B) with gradient elution at a flow rate of 0.6 mL/min, and the column temperature was 40℃. The positive ion multiple reaction monitoring(MRM) mode was used, and atmospheric pressure chemical ionization source is used as ion source The mass concentration of 6 N-nitrosamine genotoxic impurities had good linear relationships within their respective linear ranges(r2≥0.999 5). The overall recoveries were between 97.83% and 103.33%, and the RSD was 1.19%-4.45%(n=9). The LODs and LOQs were 0.033 7-0.033 89 ng/mL, 0.100 76-0.102 68 ng/mL, respectively. The established method is speci fic, simple, rapid, and sensitive, which is suitable for the determination of N-nitrosamine genotoxic impurities in metformin hydrochloride enteric-coated tablets. 
关键词:液相色谱-质谱法;盐酸二甲双胍肠溶片;基因毒性杂质 
Keywords:Liquid chromatography-mass spectrometry; metformin hydrochloride enteric-coated tablets; genotoxicimpurities 
本文引用格式:
徐艳梅,李挥,张素平,等.高效液相色谱-质谱联用法同时测定盐酸二甲双胍肠溶片中6种亚硝胺类基因毒性杂质[J].化学分析计量,2022,31(5):28.
XU Yanmei,LI Hui,ZHANG Suping,et al. Simultaneous determination of 6 nitrosamine genotoxic impurities in metformin hydrochloride enteric-coated tablets by high performance liquid chromatography-mass spectrometry[J]. Chemical Analysis and Meterage,2022,31(5):28. 

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