摘要
目的:建立白芍药材中19种有机氮类农药残留的毛细管电泳-质谱联用(CE-MS)检测方法。方法:采用CE-MS方法,熔融石英毛细管柱(70 cm×50μm),运行缓冲液为1%甲酸-15%甲醇水溶液(V/V,pH 2.2)。毛细管温度为25℃,分离电压为20 kV。质谱条件:采用电喷雾离子源(ESI),正离子模式检测;鞘液为90%甲醇-0.2%甲酸水溶液,流速为8μl.min-1;干燥气流速为6 L.min-1,干燥气温度为250℃;雾化气压力为5 psig;碎片电压为100 V,毛细管电压为5 000 V。结果:19种农药在一定浓度范围内呈线性关系,相关系数为0.9918～0.9986。19种农药的加样回收率为80.1%～108.4%,相对标准偏差(RSD)<20%(除螺环菌胺为22.3%,乙氧喹啉为29.2%外),检测限(LOD)为0.503μg.kg-1～10.1μg.kg-1。结论:该CE-MS分析方法专属性强、重现性好,适用于白芍药材中有机氮类农药的检测分析。
Objective： To establish a capillary electrophoresis-mass spectrometry（CE-MS） method for the analysis of nineteen organonitrogen pesticides in Paeoniae Radix Alba. Methods： CE-MS analysis was performed on a 70 cm×50 μm fused-silica capillary.The optimal buffer was composed of 1% formic acid and 15% methanol（V/V,pH 2.2）.The temperature of capillary was controlled at 25℃.The separation voltage was ＋20 kV.The optimal MS parameters were as follows：ESI-MS analysis was performed in the positive mode;90% methanol containing 0.2% formic acid with a flow rate of 8 μl·min-1 was selected as the sheath liquid;the flow rate and temperature of drying gas were 6 L·min-1 and 250℃,respectively;The nebulizing gas pressure was set at 5 psig;The optimal values of fragmentor and ESI voltage were 100 V and 5 000 V,respectively. Results： The nineteen pesticides had good linearity over the testing ranges.The average recoveries were in the range of 80.1%-108.4% with RSDs less than 20%（except ethoxyquin and spiroxamine,those of which were 29.2% and 22.3% at 0.01 mg·kg-1 concentration level）.The LODs of nineteen pesticides were 0.503~10.1 μg·kg-1. Conclusion： The method can be used effectively to analyze the nineteen organonitrogen pesticides residue in Paeoniae Radix Alba.
出处
《浙江大学学报（医学版）》
CAS
CSCD
北大核心
2012年第1期25-31,共7页
Journal of Zhejiang University(Medical Sciences)
基金
"重大新药创制"国家科技重大专项(No.2009ZX09502-024)
关键词
白芍/分析
电泳
毛细管
质谱分析法
有机氮类/分析
杀虫药/分析
Radix Paeoniae Alba/analysis
Electrophoresis
capillary
Mass spectrometry
Organonitrogen/analysis
Insecticides/analysis
