超高效液相色谱-串联质谱法测定食用菌中农药多残留研究

摘要

An ultra performance liquid chromatography-tandem mass spectrometric method (UPLC-MS/MS) is developed for the simultaneous determination of 10 residues in edible fungus .The pesticides were extracted with acetonitrile ,cleaned up with NH2 solid phase extraction cartridge (SPE) .The UPLC analysis are performed on an Acuity UPLC HSST3column with gradient eluation ,combining with multiple reaction monitoring (MRM ) mode .The linear range is 10-200μg/L ,the correlation coefficients is above 0.9985 in the linear range .The average recoveries of 10 pesticides in spiked fungus (0 .01 and 0 .05mg/kg) is 80 .3%-102 .6% ,and the relative standard deviation is below 9 .8% .T he results indicate that the meth-od is easier ,faster ,more sensitive and better purification effect .And the method can meet the require-ments for simultaneous determination of multi-residues in edible fungus .%采用超高效液相色谱-串联质谱（U PLC -M S/M S ）技术，建立了同时检测食用菌中10种农药的多残留检测方法。样品经乙腈提取，氨基固相萃取柱净化，Waters HSST3超高效液相色谱柱分离，进入电喷雾串联四极杆质谱进行检测，采用多反应监测（M RM ）分析，对液质分离条件和样品前处理条件进行了优化。结果表明10种农药在10～200μg/L 范围内线性良好（r≥0.9985）。在0.01、0.05 mg/kg 浓度范围内，平均加标回收率在80.3％～102.6％之间；相对标准偏差RSD （％）≤9.8％。该方法的最低检出限范围为1.72×10-4～9.28×10-3 mg/kg。该方法简便、快速、灵敏、净化效果好，测定结果满足食用菌农药多残留的检测要求。