Simultaneous determination of saflufenacil and three metabolites in five agriculture products using liquid chromatography—Tandem mass spectrometry

Abstract

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 (R2 > 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.

The Environmental Degradation and Distribution of Saflufenacil, a Fluorinated Protoporphyrinogen IX Oxidase–Inhibiting Herbicide, on a Canadian Winter Wheat Field

“…For sediment samples the percentage of recovery was determined to be 85 ± 6% ( n = 8) with a method detection limit of 5.68 ng/tube (3σ/m, n = 5). This simple extraction method, which has proved to be effective in the extraction of saflufenacil from soils, requires less time and fewer materials than other published methods for saflufenacil extraction, allowing for more samples to be processed in a shorter time with equivalent recovery and detection limits (Lan et al 2014; Wu et al 2019).…”

“…There is limited peer‐reviewed literature regarding the monitoring for transport or persistence in soils from fields where saflufenacil has been applied, a fact noted in the most recent Canadian registration decision for saflufenacil (Health Canada 2017). In one of the most recent studies (Wu et al 2019), the authors identified a new analytical methodology to detect saflufenacil and 3 metabolites in consumer agricultural products. In an earlier study, Lan et al (2014) employed an analytical extraction method to detect saflufenacil and 2 metabolites in soil samples.…”

Analytical methods to analyze pesticides and herbicides

“…Under the optimal conditions, this method achieved recoveries of 76%-97% with RSDs of 1%-9%, low LODs (0.001-41.27 ng/L), and good linearity. Wu et al (2019) established an efficient method for analyzing saflufenacil and the metabolites simultaneously in agriculture products with LC-MS/MS. The sample extraction was carried out using acetonitrile, followed by purification with Florisil or Florisil with octadecylsilane, prior to detection with Shim-pack GIST C18 column connected to an EI source.…”