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引用本文:朱荣,奉艳花,黄丽丽.GC测定那可丁中5种残留溶剂的含量[J].中国现代应用药学,2021,38(22):2787-2790.
ZHU Rong,FENG Yanhua,HUANG Lili.Determination of 5 Residual Solvents in Noscapine by GC[J].Chin J Mod Appl Pharm(中国现代应用药学),2021,38(22):2787-2790.
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GC测定那可丁中5种残留溶剂的含量
朱荣, 奉艳花, 黄丽丽
广西壮族自治区食品药品检验所, 南宁 530021
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。
关键词:  那可丁  残留溶剂  顶空进样  气相色谱法
DOI:10.13748/j.cnki.issn1007-7693.2021.22.004
分类号:R917
基金项目:“重大新药创制”国家科技重大专项(2017ZX09101001)
Determination of 5 Residual Solvents in Noscapine by GC
ZHU Rong, FENG Yanhua, HUANG Lili
Guangxi Institute for Food and Drug Control, Nanning 530021, China
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.
Key words:  noscapine  residual solvent  headspace injection  GC
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