顶空气相色谱法测定降胆固醇药YA中的残留溶剂量-现代仪器与医疗.pdf

《现代仪器与医疗》 2015年  第21卷   第1期 检验检测 顶空气相色谱法测定降胆固醇药YA中的 残留溶剂量 1 2 1 2 全红娜 　金松子 　商国举 　蒋庆峰 （1.天津中医药大学，天津　300193；2.天津药物研究院药物分析测试中心，天津　300193 ） [ 摘　要 ]　目的：建立YA 原料药中甲醇、异丙醇、二氯甲烷、乙酸乙酯、正庚烷、甲苯、乙酸丁 酯和氯苯8 种残留溶剂的测定方法。方法：采用Agilent DB-624 毛细管色谱柱（30 m ×0.53 mm ，30 µm ）；顶空进样法；FID 检测器；程序升温：40 ℃维持2 min ，5 ℃· min-1 升温至80 ℃，维持2 min ， 10 ℃·min-1 升温至200 ℃。选用二甲基亚砜为溶剂。结果：各溶剂分离情况良好，在各自的浓度范围内， 线性关系良好，8 种溶剂的平均回收率范围为96.4% ～ 101.0% ，RSD 值是0.5% ～ 2.2% 。结论：该方 法灵敏度高、简便、快速准确，可用于YA 原料药中残留溶剂的检测。 [ 关键词 ]　气相色谱法；残留溶剂；顶空进样 中图分类号: O657　文献标识码: A　文章编号：2095-5200（2015）01-067-03 DOI：10.11876/mimt201501024 Determination of residual solvents in cholesterol-lowering drugs YA by headspace GC QUAN Hong-na1 JIN Song-zi2 SHANG Guo-ju1 JIANG Qing-feng2. 1.Tianjin University of ， ， （ Traditional Chinese Medicine, Tianjin 300193,China; 2. Center for Testing and Analysis, Tianjin Institute of Pharmaceutical Research, Tianjin 300193,China ） [Abstract]　Objective: To establish a method for determination of the residues of eight kinds of residual solvents in YA by gas chromatography. Methods: The eight organic solvents were separated on a Capillary Column of DB-624 (30 m×0.53 mm,30μm); Headspace injector; FID detector; Using programmable increased temperature: the column temperature is initially maintained at 40 for 2 min and then up to 80 at the ℃ ℃ rate of 5 ℃•min-1 for 2 min, and eventually raised to 200 at the rate of 10 •min-1. Results: Each solvent ℃ ℃ was completely separated and had excellent linearity in the range of respective concentrations. The average recoveries were 96.5% to 101.0% with coefficient of variation from 0.3% to 2.2%. Conclusion: The method is sensitive, simple, rapid and accurat