GC测定那可丁中5种残留溶剂的含量

Determination of 5 Residual Solvents in Noscapine by GC

关键词:  那可丁  残留溶剂  顶空进样  气相色谱法

Key words:  noscapine  residual solvent  headspace injection  GC

摘要:

目的 建立可同时测定那可丁中5种残留溶剂的GC法。方法 以1 mol·L^-1的盐酸溶液为溶剂，采用顶空进样法，以DB-624大口径毛细管柱程度升温模式，FID检测器检测那可丁原料中甲醇、乙醇、丙酮、异丙醇、四氢呋喃5种有机溶剂残留。结果 甲醇、乙醇、丙酮、异丙醇、四氢呋喃分别在0.03~3.33，0.04~5.07，0.03~4.93，0.03~4.82，0.01~0.82 mg·mL^-1内线性关系良好，5种成分的平均回收率为98.77%~108.69%；检出限分别为0.02%，0.01%，0.004%，0.01%，0.003%。结论 本方法灵敏度高、准确性好、简便易行，可用于那可丁中有机溶剂残留的检测。

Abstract:

OBJECTIVE To establish a GC method for simultaneous determination of 5 organic solvent residues in noscapine. METHODS The sample was dissolved by 1 mol·L^-1 hydrochloric acid solution, a headspace injection method with temperature programed mode was used to determine the residual organic solvents of methanol, ethanol, acetone, isopropanol and tetrahydrofuran in noscapine crude drugs by DB-624 wide bore capillary column and FID detector. RESULTS Good linear relationships of methanol, ethanol, acetone, isopropanol and tetrahydrofuran were obtained in 0.03-3.33, 0.04-5.07, 0.03-4.93, 0.03-4.82, and 0.01-0.82 mg·mL^-1 respectively. The average recoveries of five organic solvents ranged from 98.77% to 108.69%, and the detection limits were 0.02%, 0.01%, 0.004%, 0.01% and 0.003%. CONCLUSION This method is sensitive, accurate, simple and easy to use, can be used for the determination of residual organic solvent in noscapine.