对乙酰氨基酚泡腾颗粒中间体乙醇残留量测定  

Determination of Residual Ethanol in Acetaminophen Effervescent Granules Intermediates by Headspace Gas

作　　者：黄磊 彭雅荣 王素芳 沙小婷 HUANG Lei;PENG Yarong;WANG Sufang;SHA Xiaoting(Xinjiang Yinduolan Pharmaceutical Co.LTD,Urumuqi,830010,China)

机构地区：[1]新疆银朵兰药业股份有限公司,乌鲁木齐830010

出　　处：《新疆医学》2024年第11期1307-1310,1314,共5页Xinjiang Medical Journal

基　　金：新疆维吾尔自治区重点研发计划项目(项目编号:2020B03007)

摘　　要：目的建立顶空气相色谱法测定对乙酰氨基酚泡腾颗粒中间体乙醇残留量,初步探讨某企业对乙酰氨基酚泡腾颗粒中间体乙醇残留情况。方法色谱柱为DB-624柱(30m×0.32mm,1.8μm),恒温40℃保持5min,匀速升温至250℃保持5分钟;进样口温度为200℃;检测器温度为250℃;载气为氮气,流速2.0mL/min;分流比10:1;柱流量2.0mL/min,平衡时间为30min,进样量1mL。对前述方法进行系统适用性、专属性、检测限、定量限、线性范围、加标回收率、重复性、重现性验证。结果乙醇峰理论塔板数>5000且无相邻杂质峰,空白溶液、空白辅料、稀释剂对对乙酰氨基酚泡腾颗粒中间体乙醇残留量检测没有干扰;乙醇的LOD为0.2994μg/mL,LOQ为0.9980μg/mL,回收率为102.65.36%~118.81%,重复性RSD为3.3%,中间精密度RSD为4.9%,线性回归方程为Y=1417.14X-8943.69(r=0.9979),线性范围为99.8~998.0μg/mL,3批样品乙醇残留量为0.2%-0.3%。结论本研究所建立方法操作简便,专属性强、灵敏度高,可用于对乙酰氨基酚泡腾颗粒中间体乙醇残留检测。Objective To establish a headspace gas chromatography method for the determination of residual ethanol in the intermediate of acetaminophen effervescent granules,and to preliminarily explore the residual ethanol in the intermediate of acetaminophen effervescent granules.Methods The chromatographic column was DB-624 column(30m×0.32mm,1.8μm).The column was maintained at 40℃for 5 min,and the column was heated to 250℃for 5 min.The inlet temperature was 200℃.The detector temperature was 250℃.The carrier gas was nitrogen at a flow rate of 2.0 mL/min.The shunt ratio was 10:1;the column flow rate was 2.0mL per minute,the equilibrium time was 30 minutes,and the injection volume was 1mL.The system applicability,specificity,detection limit,quantitative limit,linear range,recovery rate,repeatability and reproducibility of the above method were verified.Results Theoretical number of ethanol peaks>5000 and no adjacent impurity peaks,The blank solution,blank excipients and diluent did not interfere with the detection of acetaminophen effervescent granule intermediate;The LOD of ethanol was 0.2994μg/mL,The LOQ was 0.9980μg/mL,The recovery ranged from 102.65.36%to 118.81%,A repetitive RSD was 3.3%,The intermediate precision RSD of 4.9%,Linear regression equation is Y=1417.14X-8943.69(r=0.9979),Linear range ranged from 99.8 to 998.0μg/mL,The ethanol residue of 3 samples was 0.2%–0.3%.Conclusion The method established in this study is simple,specific and sensitive,and can be used for the detection of ethanol residue in acetaminophen effervescent granules.

关 键 词：对乙酰氨基酚 泡腾颗粒 顶空气相色谱法 乙醇 

分 类 号：R917[医药卫生—药物分析学]