Zhang Yule, Huang Chaoqun, Zhu Xiaoyu, Chen Xiaomei, Mo Weimin
College of Chemical Engineering and Material, Zhejiang University of Technology, Hangzhou 310014, China.
Se Pu. 2013 Mar;31(3):264-9. doi: 10.3724/sp.j.1123.2012.10021.
An LC-MS/MS method was developed for the simultaneously determination of seven strobilurin fungicide residues in Chinese herbs. The strobilurin fungicides include Z-metominostrobin, kresoxim-methyl, dimoxystrobin, picoxystrobin, pyraclostrobin, azoxystrobin and trifloxystrobin. The sample was extracted with ethyl acetate and cleaned-up by an amino SPE column. The seven strobilurin fungicide residues were separated on a C18 column with gradient elution of 1.0 per thousand formic acid and methanol as mobile phases, and detected by ESI-MS in positive ion and selective reaction monitoring (SRM) mode. External standard method was used to the quantification with good linear relationships (r > or = 0. 996). The LOQs were 2 micro g/kg for dimoxystrobin, picoxystrobin and trifloxystrobin, 4 mciro g/kg for pyraclostrobin and azoxystrobin, 10 micro g/kg for Z-metominostrobin and kresoxim-methyl. The recoveries were from 60.4% to 110% with the RSDs between 1.2% and 17%. The developed method is suitable for the determination and confirmation of the seven strobilurin fungicide residues in the three of Eight Zhes ( Ophiopogon japonicus (Thunb.), Scrophularia ningpoensis Hemsl. and Corydalis yanhusuo W T Wang).
建立了一种液相色谱-串联质谱法同时测定中药材中7种甲氧基丙烯酸酯类杀菌剂残留量的方法。这7种甲氧基丙烯酸酯类杀菌剂包括Z-甲氨基苯甲酰胺菌酯、醚菌酯、烯肟菌酯、啶氧菌酯、吡唑醚菌酯、嘧菌酯和肟菌酯。样品用乙酸乙酯提取，经氨基固相萃取柱净化。7种甲氧基丙烯酸酯类杀菌剂残留于C18柱上分离，以0.1%甲酸和甲醇为流动相进行梯度洗脱，采用电喷雾离子源-质谱正离子模式和选择反应监测（SRM）模式检测。采用外标法定量，线性关系良好（r≥0.996）。啶氧菌酯、啶氧菌酯和肟菌酯的定量限为2μg/kg，吡唑醚菌酯和嘧菌酯为4μg/kg，Z-甲氨基苯甲酰胺菌酯和醚菌酯为10μg/kg。回收率在60.4%～110%之间，相对标准偏差在1.2%～17%之间。该方法适用于测定和确证浙八味中的麦冬、玄参和延胡索3种中药材中7种甲氧基丙烯酸酯类杀菌剂残留量。
