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

作　　者：张晓娟 ZHANG Xiaojuan(Testing Technology Company of Changsha Research Institute of Mining and Metallurgy Co.,Ltd.,Changsha,Hunan,410012 P.R.China;Hunan Agricultural University,Changsha,Hunan,410012 P.R.China)

机构地区：[1]长沙矿冶院检测技术有限责任公司,湖南长沙410012 [2]湖南农业大学,湖南长沙410012

出　　处：《华西药学杂志》2024年第2期197-199,共3页West China Journal of Pharmaceutical Sciences

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/z 79,定性离子为m/z 81。结果1.0~5.0 mg·L^(-1)1,3-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。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 C,ionization energy of 70 eV,quadrupole temperature of 150℃C,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 

分 类 号：R917[医药卫生—药物分析学]