摘要
采用液相色谱-电喷雾串联四极杆质谱仪,用多离子反应检测(MRM)定量法检测,通过对样品SPE净化预处理、色谱条件、质谱参数等的优化选择和方法学验证,建立了定量检测止咳药中的罂粟壳含量的理想方法。吗啡、可待因、罂粟碱、那可丁的母离子质荷比分别为286.2、300.2、340.7、413.4、289.3;定量用子离子分别为165.0、215.1、202.5、324.7、220.0、201.1,另一组子离子分别为181.1、165.1、324.7、353.1、165.0。本方法灵敏度高、操作简单、定量准确。吗啡、可待因、罂粟碱、那可丁的检出限LOD分别为0.073、0.024、0.003和0.O009μg/L(进样量10μL),定量限LOQ分别是0.24、0.08、0.01和0.003μg/L。回收率为95%~110%。
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MA/MS) method for the determination of alkaloids residues in antitussive adulterated with pericarpium papaveris was described. The procedures of extraction, preparation and analysis were discussed, m/z of precursor ions for morphine, codeine, narcotine, papaverine and morphine ( D3 ) were 286.2, 300.2, 340.7, 413.4, 289.3, respectively. Daughter ions of quantitation were 165.0, 215. 1, 202.5, 324. 7, 220.0, 201. 1, respectively. Another daughter ions were 181.1, 165.1, 324.7, 353.1, 165.0, respectively. This method has the advantages of high sensitivity, accuracy and easy to operation. Limits of detection for morphine, codeine, narcotine and papaverine were 0. 073,0. 024, 0. 003, 0. 0009 μg/L 10 μL of imject volume, respectively. The limit of quantitation were 0.24, 0.08, 0.01, 0. 003 μg/L, respectively. The recoveries were 95% - 110%.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2006年第8期1175-1178,共4页
Chinese Journal of Analytical Chemistry
关键词
罂粟壳
电喷雾
三重四极杆液质联用
多离子反应检测
Pericarpium papaveris, electriospray ionization, liquid chromatography-tandedm mass spectrometry, muhiion reaction monitoring