Multivariate optimization of a new LC–MS/MS method for the determination of 156 pesticide residues in milk and dairy products

Abstract

BACKGROUND Pesticides are widely utilized worldwide to control undesirable life forms during the planting procedure in agriculture. But they can pollute the nature and jeopardize human wellbeing. Additionally, on account of high resistance and biological activity; pesticides are able to accumulate in living organs and lead to acute and long‐term negative effects along with toxicity. Milk and dairy products constitute an important part of a humans’ diet since they contain fundamental supplements and nutrients, however they may also be the source of unhealthy components including pesticides. Therefore efficient, accurate and sensitive determination methods must be improved to quantify pesticide residues in these food samples. RESULTS Multivariate optimization strategy was employed to optimize an efficient and robust liquid chromatography coupled with tandem mass spectrometry (LC–MS/MS) method for the determination of 156 pesticide residues in milk and dairy products. Three independent variables considered and their levels in the Box–Behnken design were as follows: initial percentage of eluent A in mobile phase (30, 40, 50%), flow rate of the mobile phase (0.1, 0.2, 0.3 mL min−1), and ammonium formate concentration in mobile phase (0.0, 0.5, 1.0 mmol L−1). Under optimized conditions, average recoveries of target analytes were obtained in the range of 70.38% to 119.04%. Detection and quantification limits ranged from 0.06 to 2.70 μg kg−1 and from 0.22 to 8.10 μg kg−1, respectively. CONCLUSION The validated method was successfully implemented to the analysis of 20 milk and dairy products including cream, cheese and yogurt. This method could be applied in many laboratories to reduce analysis time and cost. © 2020 Society of Chemical Industry

Development of a High-Throughput Screening Analysis for 195 Pesticides in Raw Milk by Modified QuEChERS Sample Preparation and Liquid Chromatography Quadrupole Time-of-Flight Mass Spectrometry

“…This study used acetonitrile with 1% acetate as an extraction solvent because it can extract various compounds with different polarity ranges and is the most effective organic solvent in multi-residue methods [17,18,20]. The volumes of extraction solution, such as 10 mL, 16 mL, and 20 mL of acetonitrile with 1% acetate, were compared to improve the extraction efficiency.…”

“…Therefore, to meet these requirements, there is an increasing need for an effective analytical method for simultaneous qualitative and quantitative screening of pesticide residues in milk. The current reported methods for the analysis of multiresidue pesticides in milk use different detection techniques, such as high-performance liquid chromatography with diode-array detection (HPLC-DAD) [12], gas chromatographyelectron capture detection (GC-ECD) [13], gas chromatography-mass spectrometry (GC-MS) [14], gas chromatography-tandem mass spectrometry (GC-MS/MS) [15,16], and liquid chromatography-tandem mass spectrometry (LC-MS/MS) [17][18][19]. Recently, liquid chromatography coupled with high-resolution mass spectrometry techniques (LC-HRMS) had been applied to determine pesticide residues in milk matrices [20,21].…”

“…Different sample preparation methods for extracting pesticides from milk have been explored. These methods mainly include liquid-liquid extraction (LLE) [19,24], gel permeation chromatography (GPC) [15], solid-phase extraction (SPE) [5,25], dispersive solid-phase extraction (d-SPE) [21], and the QuEChERS (quick, easy, cheap, effective, rugged, and safe) method [13,14,16,18]. Among them, GPC and SPE are tedious and time-consuming to operate, which do not facilitate the processing of a large number of samples.…”