QuEChERS-气相色谱-串联质谱法和高效液相色谱-串联质谱法快速检测蔬菜中267种香港规例中的农药残留量

Rapid determination of 267 kinds of Hong Kong regulatory pesticide residues in vegetables by QuEChERS combined with gas chromatographytandem mass spectrometry and high performance liquid chromatography-tandem mass spectrometry

目的建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry,GC-MS/MS)和高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)快速检测供港蔬菜中267种香港规例农药残留量的方法。方法样品以1%(V:V)乙酸乙腈为提取溶剂,高速匀浆提取,采用改进的QuEChERS法进行净化后,经仪器测定。结果GC-MS/MS法中添加内标磷酸三苯酯校正回收率,样品由基质匹配标准曲线进行定量,所检测的118种农药在0.01-0.20 mg/L范围内线性关系良好,相关系数均在0.995以上;HPLC-MS/MS用基质匹配标准曲线进行检测的149种农药在0.005~0.20 mg/L范围内线性关系良好,相关系数大于0.990。所有的农药定量限均小于0.01 mg/kg,各个浓度水平加标回收率为67.2%~120.7%,相对标准偏差为0.1%~17.7%(n=6)。结论本方法重现性和稳定性良好,定量限满足港澳以及世界各地对农残检测的要求,适用于供港蔬菜中农药多残留的高通量快速筛查及应急检测需要。

Objective To establish a method for determination of 267 kinds of Hong Kong regulatory pesticide residues in vegetables by QuEChERS(quick,easy,cheap,effective,rugged,and safe)combined with gas chromatography-tandem mass spectrometry(GC-MS/MS)and high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample was extracted with 1%(V:V)acetonitrile and homogenized with high speed homogenate.The sample was purified by improved QuEChERS method and measured by the instrument.Results The GC-MS/MS method added internal standard triphenyl phosphate to calibrate the recovery rate,and the samples were quantified by matrix matching standard curves.The 118 pesticides detected had good linear relationships within the range of 0.01-0.20 mg/L,and the correlation coefficients were all above 0.995.The 149 pesticides detected by HPLC-MS/MS with matrix matching standard curve had good linear relationships in the range of 0.005-0.20 mg/L,and the correlation coefficients were greater than 0.990.The limits of quantification of all pesticides were less than 0.01 mg/kg,the recovery rates of each concentration level were 67.2%-120.7%,and the relative standard deviations were 0.1%-17.7%(n=6).Conclusion The method has good reproducibility and stability,and the limits of quantification meet the requirements for pesticide residue detection in Hong Kong,Macao and other parts of the world.It is suitable for high-throughput rapid screening and emergency detection of pesticide residues in vegetables supplied to Hong Kong.