GC法测定对乙酰氨基酚口服液体制剂辅料中乙二醇及二甘醇残留量  

Determination of Ethylene Glycol,Diethylene Glycol in the Excipients of Acetaminophen Oral Liquid Preparation by GC

作　　者：黄丽梅 曹玉 戴震 仝立卿 张珂 Huang Limei;Cao Yu;Dai Zhen;Tong Liqing;Zhang Ke(Nanjing Food and Drug Supervision and Inspection Institute,Nanjing 210038,China)

机构地区：[1]南京市食品药品监督检验院,江苏南京210038

出　　处：《云南化工》2024年第8期124-127,共4页Yunnan Chemical Technology

摘　　要：目的:建立对乙酰氨基酚口服液体制剂辅料中乙二醇、二甘醇残留量的检测方法。方法:采用气相色谱法,检测器为氢火焰离子化检测器(FID),以Agilent VF-17ms(30 m×?0.53 mm,1.0μm)为色谱柱,程序升温,进样口温度为270℃,检测器温度290℃。结果:在确定的色谱条件下各主峰分离度良好;乙二醇和二甘醇分别在5.94~118.80μg/mL、5.34~106.8μg/mL的质量浓度范围内线性关系良好(r≥0.999);2者检测限分别为0.894μg/mL和0.846μg/mL,定量限分别为2.683μg/mL和2.538μg/mL;重复性的RSD均<2.0%;乙二醇回收率在95.6%~99.5%,二甘醇回收率在95.3%~97.3%。结论:方法灵敏度高,专属性和重复性良好,线性和回收率均符合2020年版《中国药典》要求,适用于检测对乙酰氨基酚口服液体制剂中的的乙二醇、二甘醇残留量检查。(Objective) To establish a method for the determination residual solvent for ethylene glycol and diethylene glycol in the excipients of acetaminophen oral liquid preparation.(Methods) Ethylene glycol and diethylene glycol were detected by gas chromatography.Hydrogen flame ionization detector(FID) were used in the method.The samples was separated on column Agilent VF-17 ms(30 m×?0.53 mm,1.0 μm) with temperature programming.The inlet temperature was 270℃,the detector temperature was 290 ℃.(Results)The method had good separation with determination of chromatographic conditions.The linear relationships of ethylene glycol and diethylene glycol were good in the concentration ranges of 5.94-118.80 μg/mL and 5.34-106.8 μg/mL(r≥0.999);The detection limits were 0.894 μg/mL and 0.846 μg/mL.The limits of quantitation were 2.683 μg/mL and 2.538 μg/mL.The RSDs of repeatability were lower than 2.0%.The recoveries of ethylene glycol and diethylene glycol were in the range of 95.6%-99.5% and 95.3%-97.3%.(Conclusion) The impurities detection methods established in this paper have good sensitivity,specificity and repeatability.The linearity and recovery are in line with the requirements of Chinese Pharmacopoeia.It is suitable for the determination of ethylene glycol and diethylene glycol in the excipients of acetaminophen oral liquid preparation.

关 键 词：对乙酰氨基酚口服液体制剂 残留溶剂 气相色谱法 乙二醇 二甘醇 

分 类 号：R927[医药卫生—药学] O657[理学—分析化学]