改进的快速QuECHERS超高效液相色谱-串联质谱法同时测定油籽和油脂中6种氨基甲酸酯类农药及其代谢物

IF 5.2 Q1 FOOD SCIENCE & TECHNOLOGY Journal of Future Foods Pub Date : 2023-06-06 DOI:10.1016/j.jfutfo.2023.05.009
Bangben Yao , Yun Li , Ru Zhang , Li Yao , Jianguo Xu , Chao Yan , Wei Chen
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引用次数: 0

摘要

基于改进的快速QuEChERS(快速、简便、廉价、有效、稳定、安全)方法,结合超高效液相色谱-串联质谱(UPLC-MS/MS),建立并验证了一种同时测定6种氨基甲酸酯类农药及其代谢产物的灵敏可靠方法。该方法还应用于23种常用油籽和油料样品的分析。样品用乙腈提取三次,然后通过250mg沉淀二氧化硅吸附剂(PSA)和250mg C18直接过滤提取的溶液。流动相为水(含0.1%甲酸)和乙腈。在优化的条件下,采用外标方案对该方法的回收率、线性、精密度、灵敏度和相对标准偏差(RSD)进行了验证。建立了具有不同范围的线性校准曲线,其中R2>;0.9973,检测限(LOD)范围为0.100µg/kg至2.000µg/kg,定量限(LOQ)范围为0.300µmg/kg至6.000µg/kg。检测限满足实际样品中最大残留限量的检测要求。同时,在10种油籽基质中,回收率为60.2%至116.6%,相关RSD为0.33%至5.35%,在13种油基质中,RSD为61.9%至116.9%,相关RSD为0.30%至5.02%。这些特性确实使UPLC-MS/MS成为精确和高通量分析复杂基质中氨基甲酸酯残留物的理想分析平台。
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Simultaneous determination of 6 carbamate pesticides and relevant metabolites in oilseeds and oil with the modified fast QuECHERS method by ultra-performance liquid chromatography-tandem mass spectrometry

A sensitive and reliable method was developed and validated for the simultaneous determination of 6 carbamate pesticides and relevant metabolites based on the modified fast QuEChERS (quick, easy, cheap, effective, rugged and safe) method combined with ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The method was also applied in the analysis of 23 commonly consumed oilseeds and oil samples. The sample was extracted with acetonitrile for three times and then the extracted solution was filtered directly through 250 mg precipitated silica adsorbent (PSA) and 250 mg C18. The mobile phase was water (containing 0.1% formic acid) and acetonitrile. The external standard protocols were adopted to validate the method in terms of recovery, linearity, precision, sensitivity, and relative standard deviation (RSD) under the optimized conditions. The linear calibration curves with different ranges were established with R2 > 0.997 3, limit of detections (LODs) ranged from 0.100 µg/kg to 2.000 µg/kg and limit of quantitations (LOQs) ranged from 0.300 µg/kg to 6.000 µg/kg. The limit of detection meets the detection requirement for the maximum residue limits in practical samples. Meanwhile, the recoveries ranged from 60.2% to 116.6% with associated RSDs ranged from 0.33% to 5.35% in 10 oilseeds matrices and ranged from 61.9% to 116.9% with RSDs ranged from 0.30% to 5.02% in 13 oil matrices. These features do make the UPLC-MS/MS an ideal analytical platform for accurate and high throughput analysis of carbamates residues in the complex matrix.

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