摘要
目的建立测定中药材中19种氨基甲酸酯农药残留量的超高效液相-串联四级杆质谱方法。方法 多反应监测模式测定,以Waters ACQUITY UPLC BEH C18进行分离,乙腈-0.1%甲酸溶液(1∶1,流速:0.2 mL·min-1。离子化模式:ESI+。结果 19种农药测定的线性范围在1.0~100.0 μg·L-1之间,r分别在0.994 7~0.999 7之间,检出质量浓度分别在0.02~0.46 μg·L-1之间, 3个水平的回收率分别在73.2%~119.7%之间。结论 该方法快速、准确、灵敏,可用于中药材中氨基甲酸酯类农药残留的测定。
Abstract
OBJECTIVE To establish a method for the determination of 19 carbamate pesticides in Chinese medicinal materials by UPLC triple-quadrupole tandem mass spectrometer. METHODS The samples were determinated by multi-reactions monitoring (MRM technology. The separation was performed on a Waters ACQUITY UPLC BEH C18 column with acetonitrile -0.1% formic acid (1∶1 with a flow rate of 0.2 mL min-1. Ion mode was set as ESI+. RESULTS The standard curves of the 19 carbamate pesticides showed good linearity over the concentration range of 1.0-100 μg·L-1 (r=0.994 7-0.999 7, respectively. The LODs of 19 carbamate pesticides were in the range of 0.02-0.46 μg·L-1 and the average recoveries were 73.2%-119.7% at three levels. CONCLUSION The method is rapid, sensitive and suitable for the determination of 19 carbamate pesticides in Chinese medicinal materials.
关键词
氨基甲酸酯 /
农药残留 /
中药材 /
超高效液相色谱 /
串联四极杆质谱
{{custom_keyword}} /
Key words
carbamate /
pesticide residues /
Chinese medicinal materials /
UPLC /
triple-quadrupole tandem mass spectrometer
{{custom_keyword}} /
张燕 杨钊 金红宇 孙磊 李欣荣 吴爱英.
UPLC-MS/MS测定中药材中19种氨基甲酸酯农药残留量[J]. 中国药学杂志, 2011, 46(3): 235-236
ZHNG Yn;YNG Zho;JIN Hong-yu;SUN Lei;LI Xin-rong;WU i-ying.
Determination of Nineteen Carbamate Pesticides in Chinese Medicinal Materials by UPLC-MS/MS[J]. Chinese Pharmaceutical Journal, 2011, 46(3): 235-236
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] LI G,YANG H J,BIAN B L.Review on the current situation of study on pesticide residue in chinese herbal medicines[J]. Chin J Exp Tradit Med Form (中国实验方剂学杂志,2005,11(4:71-73.
[2] XU Y L,LI Y K.HPLC-MS Analysis for contents of residual carbamate pesticides in a variety of Chinese herbal medicines.[ J ] . Physical Testing and Chemical Analysis(Part B:Chemical Analysis(理化检验:化学分册, 2006,42(11:877-880.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}