QuEChERS-超高效液相色谱-串联质谱法测定小麦中噻吩磺隆残留

Determination of thifensulfuron-methyl residues in Triticum aestivum L.‌ by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  噻吩磺隆  小麦  QuEChERS  超高效液相色谱串联质谱  残留分析

英文关键词:thifensulfuron-methyl  Triticum aestivum L.‌  QuEChERS  ultra performance liquid chromatography-tandem mass spectrometry  residue analysis

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定小麦中噻吩磺隆的残留。方法 样品经2%甲酸乙腈提取, 无水硫酸镁和N-丙基乙二胺替换净化, 40 ℃氮吹浓缩后, 0.1%甲酸溶液定容, UPLC-MS/MS检测, 基质匹配外标法定量。结果 在0.0005~0.0200 mg/L质量浓度范围内线性关系良好, 相关系数(r)大于0.999。在0.010~0.100 mg/kg添加回收实验中, 噻吩磺隆在小麦籽粒中的平均回收率为87%~93%, 最大相对标准偏差(relative standard deviation, RSD)为6.1%。检出限为14.37 ng/L, 定量限为47.90 ng/L。表明该方法的准确度和精密度均符合残留分析的要求。结论 该分析方法简单高效, 灵敏度较高, 有助于提高噻吩磺隆的农药的残留风险监测水平。

英文摘要:

      Objective To establish a method for determination the thifensulfuron-methyl residues in Triticum aestivum L.? by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were extracted with 2% formic acid-acetonitrile, purified by anhydrous magnesium sulfate and primary secondary amine, concentrated under nitrogen stream at 40 °C, reconstituted in 0.1% formic acid solution, and analyzed by UPLC-MS/MS. Quantification was performed by the matrix-matched external standard method. Results The method exhibited excellent linearity in the mass concentration range of 0.0005–0.0200 mg/L, with a correlation coefficient (r)>0.999. In recovery tests at spiking levels of 0.010–0.100 mg/kg, the average recoveries of thifensulfuron-methyl in Triticum aestivum L.? grains ranged from 87% to 93%, with a maximum relative standard deviation (RSD) of 6.1%. The limit of detection was 14.37 ng/L and the limit of quantitation was 47.90 ng/L. It was demonstrated that the accuracy and precision of the method met the requirements for residue analysis. Conclusion This analytical method is simple, efficient and highly sensitive, thereby enhancing the monitoring capacity for pesticide residue risks associated with thifensulfuron-methyl.