顶空毛细管气相色谱法测定龙胆泻肝片中残留溶剂  

Determination of Residual Solvents in LongdanXiegan Tablets by Headspace Capillary Gas Chromatography

作　　者：尹兴章 谭冬梅 张远溪 赵一丁 杨深应 王健芬 Yin Xingzhang;Tan Dongmei;Zhang Yuanxi;Zhao Yiding;Yang Shenying;Wang Jianfen(Baoshan Inspection and Testing Center for Food and Drug,Baoshan 678000,China;Yunnan University of Economics Management,Kunming 650000,China;Baoshan College of Traditional Chinese Medicine,Baoshan 678000,China)

机构地区：[1]保山市食品药品检验检测中心,云南保山678000 [2]云南经济管理学院,云南昆明650000 [3]保山中医药高等专科学校,云南保山678000

出　　处：《云南化工》2024年第7期114-117,共4页Yunnan Chemical Technology

摘　　要：目的:旨在建立一种新方法测定龙胆泻肝片中甲醇、乙醇的有机溶剂残留量。方法:采用顶空毛细管气相色谱法,色谱柱为安捷伦DB-624毛细管色谱柱(30 m×∅0.53 mm,3μm);检测条件为:程序升温;进样口温度为220℃;检测器(FID)温度为250℃;分流进样,选择5∶1的分流比;顶空瓶平衡温度85℃,平衡时间20 min。结果:甲醇、乙醇两种有机溶剂分离效果良好,分别在1.0335~248.04μg·mL^(-1)(r=0.9997)、1.0505~252.12μg·mL^(-1)(r=0.9996)范围内有与峰面积良好的线性关系,平均回收率分别为97.4%(RSD=1.7%,n=6)、95.7%(RSD=1.6%,n=6)。结论:方法重复性、精密度和回收率较好,而且操作简便、灵敏度高、选择性强,可为龙胆泻肝片残留溶剂质量控制提供参考依据。(Objective)The aim is to establish a new method to determine the organic solvent residues of methanol and ethanol in Longdan Xiegan tablets.(Methods)Headspace capillary gas chromatography was used,and the column was an Agilent DB-624 capillary column(30 m×∅0.53 mm,3μm);the detection conditions were:programmed temperature rise;inlet temperature was 220℃;detector(FID)temperature was 250℃;split injection,5∶1 split ratio was selected;headspace vial equilibration temperature was 85℃,equilibration time was 20 min.(Results)The two organic solvents,methanol and ethanol,were well separated with good linearity in the ranges of 1.0335~248.04μg·mL^(-1)(r=0.9997)and 1.0505~252.12μg·mL^(-1)(r=0.9996),respectively,and the average recoveries were 97.4%(RSD=1.7%,n=6),95.7%(RSD=1.6%,n=6).(Conclusion)The method has good repeatability,precision and recovery,and is simple,sensitive and selective,which can provide a reference basis for the quality control of residual solvents of gentian diarrhea liver tablets.

关 键 词：龙胆泻肝片 甲醇 乙醇 残留溶剂 顶空毛细管色谱法 

分 类 号：O657.71[理学—分析化学]