气相色谱法测定复方门冬维甘滴眼液中三氯叔丁醇的含量  

Determination of chlorobutanol in Compound Aspartate,Vitamin B_(6) and Dipotassium Glycyrrhetate Eye Drops by gas chromatography

作　　者：段希英 吴珺 徐佳 DUAN Xiying;WU Jun;XU Jia(Taizhou Institute for Drug Control,Taizhou 225300,China)

机构地区：[1]泰州市药品检验院,江苏泰州225300

出　　处：《中国药品标准》2021年第5期454-457,共4页Drug Standards of China

摘　　要：目的:建立气相色谱法测定复方门冬维甘滴眼液中三氯叔丁醇的含量。方法:色谱柱为DB-WAX毛细管柱(30 m×0.320 mm,0.50μm);采用程序升温;进样口温度:220℃;检测器温度:250℃;载气:氮气;柱流量:1.5mL·min^(-1);进样量:1.0μL;内标物为N,N-二甲基甲酰胺,溶剂为甲醇。结果:三氯叔丁醇在0.03~0.30 mg·mL^(-1)的范围内,其峰面积与浓度呈良好线性关系,Y=7.1204X-0.01878,r=0.9997;低、中、高三个浓度的加样回收率分别为101.1%、103.3%、104.5%;定量限为1.5×10^(-6)mg·mL^(-1);重复性和中间精密度的RSD分别为0.54%、1.20%。复方门冬维甘滴眼液(批号18K141、20D031及20E231)中三氯叔丁醇含量分别为2.00、2.02及2.01 mg·mL^(-1)。结论:经方法学验证,本文建立的气相色谱测定法可用于测定复方门冬维甘滴眼液中抑菌剂三氯叔丁醇的含量。Objective:To establish a gas chromatographic method for determination of chlorobutanol in Compound Aspartate,Vitamin B 6 and Dipotassium Glycyrrhetate Eye Drops.Methods:The test was performed in DB-WAX capillary column(30 m×0.320 mm,0.50μm)under the programmed temperature procedure.The injection temperature was 220℃and the detector temperature was 250℃.The carrier gas was nitrogen and the flow rate was 1.5 mL·min^(-1).The injection volume was 1μL,the internal standard was N,N-dimethylformamide,and methanol was used as the solvent.Results:The linear range of chlorobutanol fell into 0.03-0.30 mg·mL^(-1) and the linear equation was Y=7.1204X-0.01878 with r=0.9997.The spiked recovery rates of low,medium and high concentrations were 101.1%,103.3%and 104.5%,respectively.The limit of quantification was 1.5×10-6 mg·mL^(-1).The RSDs of repeatability and intermediate precision were 0.54%and 1.20%respectively.The contents of chlorobutanol in Compound Aspartate,Vitamin B 6 and Dipotassium Glycyrrhetate Eye Drops(batch numbers 18K141,20D031 and 20E231)were 2.00,2.02 and 2.01 mg·mL^(-1) respectively.Conclusion:The established gas chromatography method is validated and is suitable for the assay of chlorobutanol in Compound Aspartate,Vitamin B 6 and Dipotassium Glycyrrhetate Eye Drops.

关 键 词：复方门冬维甘滴眼液 三氯叔丁醇 气相色谱法 含量测定 

分 类 号：R921.2[医药卫生—药学]