State Key Laboratory for Biology of Plant Disease and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing, P. R. China.
Plant Protection College, Shenyang Agricultural University, Shenyang, P. R. China.
J Food Biochem. 2019 Apr;43(4):e12778. doi: 10.1111/jfbc.12778. Epub 2019 Jan 31.
A reliable and efficient method was firstly established for the simultaneous determination of saflufenacil and its metabolites (M800H02, M800H11 and M800H35) in cereals (soybean and corn) and fruits (apple, grape and orange), based on a triple quadrupole liquid chromatography mass spectrometer. The four target compounds were extracted with acetonitrile and purified by Florisil or Florisil with octadecylsilane from the cereals and fruits. Determination of the targets was achieved within 3.5 min by using Shim-pack GIST C18 column connected to an electrospray ionization source (ESI mode). The method showed excellent linearity (R > 0.9984), and the limits of quantitation were 1 µg/kg for all compounds. Average recoveries were in the range of 74.6%-108.1%, with an intra-day relative standard deviation between 0.9% and 18.3%. The inter-day relative standard deviation was less than 13.8%. The results demonstrate that this method is convenient for monitoring the residues of saflufenacil and its metabolites in food matrices. PRACTICAL APPLICATIONS: Saflufenacil controls many common annual broadleaf weed efficiently, it has been developed and launched into the market by domestic enterprises. Consequently, an analysis method for monitoring saflufenacil in food sample will be urgently needed in China over the next few years. This method provides separation with good specificity within 3.5 min, which is less than previous studies. For the five matrixes, the method presented satisfactory validation parameters in terms of good linearity, low limit of quantitations, and satisfactory accuracy and precision. Therefore, the method established in this study is a valuable tool to overcome gaps in determining saflufenacil and its metabolites in cereals and fruits, in order to accurate evaluation of risk and ensure food safety.
本研究建立了一种基于三重四极杆液质联用仪同时测定谷物(大豆和玉米)和水果(苹果、葡萄和橙子)中杀草氟苯和其代谢物(M800H02、M800H11 和 M800H35)的可靠、高效方法。四种目标化合物均采用乙腈提取,谷物和水果中的目标化合物用弗罗里硅土或弗罗里硅土-十八烷基硅烷净化。采用 Shim-pack GIST C18 柱,以电喷雾电离源(ESI 模式)进行测定,四种目标化合物在 3.5min 内均能达到良好的分离效果。该方法具有良好的线性(R>0.9984),定量限均为 1μg/kg。平均回收率在 74.6%~108.1%之间,日内相对标准偏差在 0.9%~18.3%之间。日间相对标准偏差小于 13.8%。结果表明,该方法方便快捷,可用于监测食品基质中杀草氟苯及其代谢物的残留量。
杀草氟苯能有效防治多种常见的一年生阔叶杂草,已被国内企业开发并推向市场。因此,未来几年,中国将急需建立一种监测食品样品中杀草氟苯残留的分析方法。该方法在 3.5min 内可获得良好的特异性分离,明显快于以往的研究。对于五种基质,该方法在良好的线性、低定量限、令人满意的准确度和精密度方面表现出令人满意的验证参数。因此,本研究建立的方法是克服谷物和水果中杀草氟苯及其代谢物检测空白的有效工具,为准确评估风险和确保食品安全提供了有力支持。