GC-MS法测定奥硝唑原料药中的1,3-二氯-2-丙醇
Determination of 1,3-dichloro-2-propyl alcohol residues in Ornidazole by GC-MS
张晓娟1
作者信息
- 1. 长沙矿冶院检测技术有限责任公司,湖南长沙 410012;湖南农业大学,湖南长沙 410012
- 折叠
摘要
目的 采用GC-MS法检测奥硝唑原料药中1,3-二氯-2-丙醇(1,3-DCP)的含量.方法 采用100％聚乙二醇(PEG-20M)为固定液的毛细管柱,程序升温进行分离.质谱采用电子轰击电离源(EI)电离,离子源温度230℃,离子化能量70 eV,四极杆温度150℃,质量扫描范围为40～450 amu,1,3-DCP的定量离子为m/z79,定性离子为m/z 81.结果 1.0～5.0 mg·L-11,3-DCP与峰面积的线性关系良好,检测限和定量限分别为0.2489、0.7716 mg·L-1,精密度、稳定性试验满足检测要求,加样回收率为92.48％～98.39％,RSD均小于5.0％.测定的27批奥硝唑原料药中的10批所含1,3-DCP超过了限值,其余均符合要求.结论 所用方法操作简单、结果准确、灵敏度高、重复性良好,可用于奥硝唑原料药中1,3-DCP残留量的测定.
Abstract
OBJECTIVE To detect the 1,3-dichloro-2-propanol(1,3-DCP)in Ornidazole by GC-MS.METHODS The capillary column with 100％polyethylene glycol(PEG-20M)as fixed liquid was used for separation.Mass spectrometry adopted electron bombardment ionization source(EI)ionization,ion source temperature of 230 ℃,ionization energy of 70 eV,quadrupole temperature of 150 ℃,mass scanning range of 40-450 amu,1,3-DCP quantitative ion of m/z 79,and qualitative ion of m/z 81.RESULTS The linear relationship of 1,3-DCP was good in the concentration range of 1.0-5.0 mg·L-1,and the limit of detection and limit of quantitation were 0.2489 and 0.7716 mg·L-1,respectively.The recoveries were 92.48％-98.39％with RSDs less than 5.0％.The method was used to determine 1,3-DCP in 27 batches of ornidazole raw materials,among which 10 batches of Ornidazole raw materials contained 1,3-DCP exceeded the limit value,and the rest met the requirements.CONCLUSION The method is simple,accurate,sensitive and reproducible,which can be used for the determination of 1,3-DCP residue in ornidazole.
关键词
奥硝唑/原料药/1,3-二氯-2-丙醇/残留量/气相色谱-质谱法Key words
Ornidazole/API/1,3-dichloro-2-propanol/The amount of residue/Gas chromatography-mass spectrometry引用本文复制引用
出版年
2024
NETL
NSTL
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