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自动QuEChERS结合UPLC-MS/MS测定莲雾中苯并咪唑类农药残留

Detection of Benzimidazoles Pesticide Redidues in Wax Apple by Automatic QuEChERS Combined with UPLC-MS/MS

  • 摘要: 为了建立自动QuEChERS结合高效液相色谱-串联质谱法测定莲雾中多菌灵、噻菌灵、苯菌灵及甲基硫菌灵4种苯并咪唑类农药残留量的检测方法。将莲雾样品采用混合试剂(5.5 g硫酸镁+1.5 g氯化钠+1.0 g柠檬酸钠+0.5 g柠檬酸二钠)进行净化,经QuEChERS自动样品制备系统进行制备后,应用超高效液相色谱-三重四级杆串联质谱法进行分析。结果表明,4种农药在1.00~10.00 ng/mL质量浓度范围内线性关系良好,决定系数(R2)均大于0.99;0.1、1.0、5.0 mg/kg 3个添加水平下,在莲雾基质中添加回收率为84%~105%,相对标准偏差为0.8%~9.5%(n=3),方法检出限和定量限分别为0.1~0.5μg/kg和0.5~10.0μg/kg。综上,该方法简便省时,净化效果好,灵敏度及准确度高,可用于同时测定莲雾中多菌灵、噻菌灵、苯菌灵及甲基硫菌灵4种苯并咪唑类农药的残留量。

     

    Abstract: To establish a method for the detection of four benzimidazoles pesticide redidues in wax apple, including carbendazim, thiabendazole, benomyl and thiophanate-methyl by automatic QuEChERS method combined with liquid chromatography-triple quadrupole tandem mass spectrometry(LC-MS/MS), the wax apple samples were purified with a mixed reagent(5.5 g magnesium sulfate, 1.5 g sodium chloride, 1.0 g sodium citrate and 0.5 g disodium citrate), and then prepared by QuEChERS automated sample preparation system, finally detected by liquid chromatography-triple quadrupole tandem mass spectrometry. The results showed that a good linear relationship was obtained between 4 pesticides in the concentration range of 1.00~10.00 ng/mL, and the correlation coefficient were higher than 0.99. At the three addition levels of 0.1, 1.0, 5.0 mg/kg, the addition recovery rates of wax apple samples were 84%~105% with a the relative standard deviation of 0.8%~9.5%(n=3). The detection limit and quantification limit of the method were 0.1~0.5 μg/kg and 0.5~10.0 μg/kg, respectively. In conclusion, this method is simple and time-saving, with good purification effect, high sensitivity and accuracy. It can be used for the determination of the four benzimidazoles pesticides residues including carbendazim, thiabendazile, benomyl and thiophanate-methyl in wax apple.

     

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