四唑虫酰胺及其代谢物BCS-CQ63359在番茄中的消解规律与储藏稳定性研究

Study on digestion rule and storage stability of tetraniliprole and its metabolite BCS-CQ63359 in tomato

中文关键词:  四唑虫酰胺  代谢物  消解  储藏稳定性  超高效液相色谱-串联三重四极杆质谱法

英文关键词:tetraniliprole  metabolite  dissipation  storage stability  ultra performance liquid chromatography -tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联三重四极杆质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测番茄中四唑虫酰胺及其代谢物BCS-CQ63359的分析方法, 并对四唑虫酰胺和BCS-CQ63359在番茄中的消解与储藏稳定性进行研究。方法 样品用乙腈涡旋提取, 经N-丙基乙二胺(primary secondary amine, PSA)和无水硫酸镁净化后, 取上清液离心, 过0.22 ?m滤膜, 采用BEH C18色谱柱分离, 正电离模式下由UPLC-MS/MS测定。结果 在0.001~0.500 μg/mL的质量浓度范围内, 四唑虫酰胺和BCS-CQ63359进样浓度与峰面积呈现良好的线性关系, 相关系数为0.9993~0.9999, 四唑虫酰胺和BCS-CQ63359检出限分别为0.001和0.002 mg/kg, 定量限为0.005 mg/kg。四唑虫酰胺和BCS-CQ63359的回收率为97%~106%, 相对标准偏差为2%~4%。田间试验结果表明, 四唑虫酰胺在番茄中的降解半衰期为1.3~4.4 d, 而-20 ℃条件下四唑虫酰胺和BCS-CQ63359储藏365 d平均降解率为2%和-8%。 结论 该方法的灵敏度、准确度和精密度符合农药残留分析要求。自然条件下, 四唑虫酰胺在番茄中的降解很快。根据农药残留储藏稳定性试验准则, 四唑虫酰胺和BCS-CQ63359在番茄中储藏365 d是稳定的。

英文摘要:

      Objective To establish a method for the determination of tetraniliprole and its metabolite BCS-CQ63359 in tomato by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), and study the digestion and storage stability of tetraniliprole and BCS-CQ63359 in tomato. Methods The samples were extracted by acetonitrile vortex, purified by primary secondary amine (PSA) and anhydrous magnesium sulfate, and the supernatant was centrifuged, filtered through 0.22 μm filter membrane, separated by BEH C18 chromatographic column, and determined by UPLC-MS/MS in positive ionization mode. Results Within the mass concentration range of 0.001?0.500 μg/mL, the injection concentration of tetraniliprole and BCS-CQ63359 showed a good linear relationship with the peak area, and the correlation coefficients were 0.9993?0.9999, the limits of detection of tetraniliprole and BCS-CQ63359 were 0.001 and 0.002 mg/kg, the limits of quantitation were 0.005 mg/kg, respectively. The recoveries of tetraniliprole and BCS-CQ63359 were 97%?106%, and the relative standard deviations were 2%?4%. Field test results showed that the degradation half-life of tetraniliprole in tomato was 1.3?4.4 d, while the average degradation rates of tetraniliprole and BCS-CQ63359 in storage at ?20 ℃ for 365 d were 2% and -8%. Conclusions The sensitivity, accuracy and precision of this method meet the requirements of pesticide residue analysis. Under natural conditions, the degradation of tetraniliprole in tomato is very fast. According to the pesticide residue storage stability test guidelines, tetraniliprole and BCS-CQ63359 are stable when stored in tomato for 365 d.