GC同时测定水合氯醛灌肠剂中二氯乙酸和三氯乙酸  

Simultaneous determination of dichloroacetic acid and trichloroacetic acid in chloral hydrate enemas by GC

作　　者：云琦 吴小青 袁子惠 马小华 陶亮 YUN Qi;WU Xiaoqing;YUAN Zihui;MA Xiaohua;TAO Liang(Xinjiang Tefeng Pharmaceutical Co.,Ltd.,Urumqi 830063,China;Center for Drug Evaluation and Inspection of Xinjiang,Urumqi 830011,China)

机构地区：[1]新疆特丰药业股份有限公司,新疆维吾尔自治区乌鲁木齐830063 [2]新疆维吾尔自治区药品审评查验中心,新疆维吾尔自治区乌鲁木齐830011

出　　处：《中国药品标准》2022年第6期581-586,共6页Drug Standards of China

基　　金：国家重大新药创制科技重大专项(编号:2018ZX09721003-007-010)。

摘　　要：目的:建立测定水合氯醛灌肠剂中潜在致癌杂质二氯乙酸和三氯乙酸含量的分析方法。方法:采用毛细管气相色谱法,检测器:ECD;检测器温度:250℃;进样口温度:210℃;色谱柱温度:程序升温;载气:氮气;供试品酯化衍生后直接进样。结果:检查方法专属性、准确度、重复性、线性与范围、耐用性均良好,二氯乙酸和三氯乙酸定量限分别为0.202μg·mL^(-1)(RSD为5.04%)和0.218μg·mL^(-1)(RSD为3.76%)。特丰制药和日本ESCRE水合氯醛灌肠剂二氯乙酸测定结果分别为26.22~29.93μg·g^(-1)和38.20~53.44μg·g^(-1),三氯乙酸测定结果分别为114.99~135.87μg·g^(-1)和242.75~323.36μg·g^(-1),日本制剂杂质含量更高。结论:本方法准确可靠,灵敏度高,可用于水合氯醛灌肠剂的质量控制。Objective:To establish a method for the determination of dichloroacetic acid and trichloroacetic acid in chloral hydrate enema.Methods:Capillary gas chromatography,detector:ECD;detector temperature:250℃;injection port temperature:210℃;column temperature:programmed temperature;carrier gas:nitrogen;the test sample was directly injected after esterification and derivatization.Results:The specificity,accuracy,repeatability,linearity,range,and robustness of the method were checked.The limits of quantification for dichloroacetic acid and trichloroacetic acid were 0.202μg·mL^(-1) with RSD as 5.04%and 0.218μg·mL^(-1) with RSD as 3.76%,respectively.The test results of Tefeng Pharmaceutical and Japan′s ESCRE chloral hydrate enema for dichloroacetic acid were 26.22-29.93μg·g^(-1) and 38.20-53.44μg·g^(-1),respectively.The test results of trichloroacetic acid were 114.99-135.87μg·g^(-1),242.75-323.36μg·g^(-1) respectively.The impurity content of Japanese preparations was higher.Conclusion:The method is accurate,reliable,and sensitive,and can be used for the quality control of chloral hydrate enema.

关 键 词：气相色谱法 水合氯醛灌肠剂 致癌物 二氯乙酸 三氯乙酸 

分 类 号：R921.2[医药卫生—药学]