QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留
Determination of Thirteen Pesticides in Edible Mushrooms by QuEChERS with UPLC MS/MS
-
摘要: 目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0 g用乙腈-水(4:1)15 mL超声提取,经N-丙基乙二胺(PSA)30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5~200 μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3)0.03~0.3 μg/kg。加标回收率84.3%~102%,相对标准偏差(n=6)2.8%~6.3%。结论:该方法可用于食用菌中13种农药残留的检测。Abstract: Objective:Determination of thirteen pesticides in edible mushrooms by QuEChERS with UPLC MS/MS. Methods:5.0 g sample was extracted ultrasonically for 5 min with 15 mL of 4:1 acetonitrile and water. The extract was purified by N-propyl ethylenediamine (PSA) 30.0 mg, anhydrous Magnesium sulfate 15.0 mg dispersive solid-phase extraction adsorbent.The purified solution was separated by UPLC using HSS T3 column, 0.1% formic acid and acetonitrile as mobile phase in gradient elution. Positive ESI and MRM were adopted in MS analysis. Results:Linear relationships were found between the peak area and the mass concentration of 13 pesticides within 0.5~200 μg/L. With detection limits (S/N=3) in the range of 0.03~0.3 μg/kg, recovery rates obtained by standard addition method ranged from 84.3% to 102% and RSDs (n=6) were in the range of 2.8%~6.3%. Conclusion:The proposed method was successfully applied to the detection of 13 pesticides in mushrooms.
下载: