Determination of 107 Pesticide Residues in Wolfberry with Acetate-buffered Salt Extraction and Sin-QuEChERS Nano Column Purification Coupled with Ultra Performance Liquid Chromatography Tandem Mass Spectrometry

Abstract

A multi-residue method for the determination of 107 pesticide residues in wolfberry has been developed and validated. Similar pretreatment approaches were compared, and the linearity, matrix effect, analysis limits, precision, stability and accuracy were validated, which verifies the satisfactory performance of this new method. The LODs and LOQs were in the range of 0.14–1.91 µg/kg and 0.46–6.37 µg/kg, respectively. The recovery of analytes at three fortification levels (10 µg/kg, 50 µg/kg, 100 µg/kg) ranged from 63.3–123.0%, 72.0–118.6% and 67.0–118.3%, respectively, with relative standard deviations (RSDs) below 15.0%. The proposed method was applied to the analysis of fifty wolfberry samples collected from supermarkets, pharmacies and farmers’ markets in different cities of Shandong Province. One hundred percent of the samples analyzed included at least one pesticide, and a total of 26 pesticide residues was detected in fifty samples, which mainly were insecticides and bactericide. Several pesticides with higher detection rates were 96% for acetamiprid, 82% for imidacloprid, 54% for thiophanate-methyl, 50% for blasticidin-S, 42% for carbendazim, 42% for tebuconazole and 36% for difenoconazole in wolfberry samples. This study proved the adaptability of the developed method to the detection of multiple pesticide residues in wolfberry and provided basis for the research on the risks to wolfberry health.

Analytical methods to analyze pesticides and herbicides

“…Application of Sin‐QuEChERS in 100 batches of oilseeds showed LODs of 0.006–0.054 mg/kg. Similar methodology was also reported by Chen, Lian, et al (2019).…”

Determination of 31 pesticide residues in wolfberry by LC-MS/MS and dietary risk assessment of wolfberry consumption

“…The QuEChERS (quick, easy, cheap, effective, rugged and safe) method has been broadly applied for the analysis of pesticide multi-residues in fruits and vegetables because of its simplicity, low cost, speed and broad applicability to a wide range of analytes (Anastassiades et al, 2003). At present, there are few methods for simultaneous determination of pesticide residues in wolfberry by LC-MS/MS (Chen et al, 2019). In particular, there are a few studies on the risk assessment of pesticide residues in wolfberry.…”

Quality standard of traditional Chinese medicines: comparison between European Pharmacopoeia and Chinese Pharmacopoeia and recent advances

“…Zeng et al employed UHPLC-triple quadrupole-MS/MS to determine 20 major constituents including salvianolic acids, tanshinones, flavonoids and triterpenes in different parts of Salvia miltiorrhiza [ 52 ]. Furthermore, other than active components determination, LC–MS has also been applied in analysis of toxins such as pesticide residue [ 53 , 54 ] and mycotoxins [ 55 – 57 ]. In ChP, LC–MS has been used for the test of adonifoline, a toxic alkaloid in Senecionis Scandentis Herba.…”

“…[52]. Furthermore, other than active components determination, LC-MS has also been applied in analysis of toxins such as pesticide residue [53,54] and mycotoxins [55][56][57]. In ChP, LC-MS has been used for the test of adonifoline, a toxic alkaloid in Senecionis Scandentis Herba.…”