超高效液相色谱串联质谱法同时测定蔬菜中12种新烟碱类农药残留量  

Simultaneous Determination of 12 Neonicotinoid Pesticide Residues in Vegetables by UPLC-MS/MS

作　　者：尹丹阳[1] 解宇菲 胡佳薇[1] 赵迪 YIN Danyang;XIE Yufei;HU Jiawei;ZHAO Di(Center for Disease Control and Prevention of Shaanxi Province,Xi′an,Shaanxi,China 710054)

机构地区：[1]陕西省疾病预防控制中心,陕西西安710054

出　　处：《中国药业》2024年第21期67-71,共5页China Pharmaceuticals

摘　　要：目的建立同时测定蔬菜中12种新烟碱类农药残留量的超高效液相色谱串联质谱法(UPLC-MS/MS)法。方法采用乙腈提取样品,经N-丙基乙二胺(PSA)、石墨化炭黑(GCB)基质分散净化进行预处理。色谱柱为Waters Acquity HSS T_(3)柱(100 mm×2.1 mm,1.8μm),流速为0.3 mL/min,流动相为甲醇-水(梯度洗脱),柱温为40℃,进样量为2μL;质谱分析采用电喷雾正离子多反应监测(MRM)模式,电喷雾电压为4500 V,气帘气压力为40 psi,雾化气压力为60 psi,辅助气压力为60 psi,离子源温度为550℃。采用空白基质外标法定量测定20份陕西省市售蔬菜中12种新烟碱类农药的残留量。结果12种新烟碱类农药在各自质量浓度范围内与峰面积线性关系良好(r>0.994);检测限为0.2~2.0μg/kg,定量限为0.5~3.0μg/kg;精密度试验的RSD均小于3.5%(n=6);加样回收率为82.42%~102.06%,RSD为2.12%~4.76%(n=6);基质效应为0.83~0.96。20份蔬菜样品中,检出阳性样品13份,其中,8份检出噻虫胺(0.83~67.92μg/kg),9份检出噻虫嗪(0.84~87.22μg/kg),4份检出啶虫脒(5.78~98.40μg/kg),3份检出吡虫啉(14.12~42.34μg/kg),3份检出烯啶虫胺(3.88~192.00μg/kg),2份检出呋虫胺(3.58,10.12μg/kg),1份检出氯噻啉(5.76μg/kg)。结论所建立的方法灵敏度高、准确性好,可用于蔬菜中12种新烟碱类农药的残留量测定。Objective To establish an ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS/MS)method for the simultaneous determination of 12 neonicotinoid pesticide residues in vegetables.Methods The sample was extracted with acetonitrile and pre-treated with primary secondary amine(PSA) and graphitized carbon black(GCB) matrix dispersion purification.The chromatographic column was Waters Acquity HSS T3 column (100 mm×2.1 mm,1.8μm),the flow rate was0.3 mL/min,the mobile phase was methanol-water (gradient elution),the column temperature was 40℃,and the injection volume was 2μL.Mass spectrometry analysis adopted the multi-reaction monitoring (MRM) mode with positive electrospray ionization(ESI+).The electric spray voltage was 4500 V,the air curtain pressure was 40 psi,the atomizing gas pressure was 60 psi,the auxiliary gas pressure was 60 psi,and the ion source temperature was 550℃.The quantitative determination of residues of12 neonicotinoid pesticides in 20 kinds of vegetables sold in Shaanxi Province was conducted by the blank matrix external standard method.Results The 12 neonicotinoid pesticides showed a good linear relationship with peak area within their respective mass concentration ranges (r>0.994).The limit of detection (LOD) was in the range of 0.2-2.0μg/kg,and the limit of quantification (LOQ) was in the range of 0.5-3.0μg/kg.The RSD of the precision test was all lower than 3.5%(n=6).The recovery rate of 12 neonicotinoid pesticides was in the range of 82.42%-102.06%with the RSD of 2.12%-4.76%(n=6).The matrix effect was in the range of 0.83-0.96.Among the 20 kinds of vegetable samples,13 samples were found to be positive,including eight samples with thiamethoxam (0.83-67.92μg/kg),nine samples with thiamethoxam (0.84-87.22μg/kg),four samples with imidacloprid (5.78-98.40μg/kg),three samples with imidacloprid (14.12-42.34μg/kg),three samples with imidacloprid (3.88-192.00μg/kg),two samples with fipronil (3.58-10.12μg/kg),and one sample with chlorothiacloprid (5.76μg/kg).Conclusion T

关 键 词：超高效液相色谱串联质谱法 新烟碱类农药 蔬菜 QuEChERS法 残留量测定 

分 类 号：R917[医药卫生—药物分析学]