Determination of eight endocrine disruptor pesticides in bovine milk at trace levels by dispersive liquid‐liquid microextraction followed by GC‐MS determination

Abstract

Endocrine disrupting chemicals are chemicals that interfere with any aspect of the endocrine system. Several natural and synthetic chemicals, including pesticides, have been identified as endocrine disruptors, which potentially inhibit the reproductive activity of the hormonal system. The pervasive occurrence with trace level concentrations and extensive variety are the reported characteristics of these chemicals. In this study, a dispersive liquid‐liquid microextraction method coupled with gas chromatography and mass spectrometry for the determination of eight potential endocrine disruptor pesticides (Lindane, Diazinon, Fenitrothion, Malathion, Aldrin, α‐Endosulfan, β‐Endosulfan, Methoxychlor) in bovine milk samples was developed. Several parameters that can influence the extraction efficiency were studied. Under optimized conditions, the calibration curves of all eight analytes presented coefficient of determination higher than 0.998 (range level of 2.0‐1000 ng/mL). The limits of detection and quantification ranged from 0.90 to 5.00 ng/mL and 2.50 to 15.0 ng/mL, respectively.

Detection of multiple endocrine‐disrupting chemicals in milk: Improved and safe high performance liquid chromatography tandem mass spectrometry method

“…The calibration curve was constructed by plotting a graph of the peak area and the analyte concentration, and the calibration curve equation and the coefficient of correlation ( R 2 > 0.99) were calculated for each EDC. Precision and repeatability were determined for six replicated pooled samples of each milk matrix spiked with the EDCs at concentrations 1, 2, and 5 times the LOQ [14]. The LOD and LOQ values were calculated based on signal‐to‐noise (S/N) ratios of at least 3 and 10, respectively.…”

Recent Advances in the Chromatographic Analysis of Emerging Pollutants in Dairy Milk: A Review (2018–2023)

“…Melamine was extracted from milk via DLLME by Vaseghi Baba et al before subsequent analysis using HPLC-UV, an extraction method that resulted in satisfactory relative recovery rates ranging from 79.6 to 105.0% [ 49 ]. Additionally, a study conducted by Sharma et al revealed the applicability of DLLME for the extraction of eight pesticides from milk, with a recovery rate within a range from 86.15 to 112.45% [ 81 ].…”

“…In response to these risks, international regulatory authorities have set MRLs for pesticide residues in milk in order to ensure public health. Numerous studies have been conducted to investigate and quantify the levels of pesticide residues in dairy milk by employing chromatographic techniques [ 31 , 81 , 92 , 163 ]. Table 3 offers a comprehensive summary of these key publications published in the time period of 2018–2023.…”

Synthesis of Isotopic Labelled Paracetamol Benzoate‐d3 and Its Application in the Determination of Paracetamol

“…Dispersive liquid‐liquid microextraction (DLLME) is known to be one of the most popular liquid phase microextraction methods in which a water immiscible solvent (extraction solvent) is introduced into the sample solution with the help of a solvent (dispersive solvent) being miscible with both aqueous and organic phases [20] . DLLME has a wide application area from pesticides [21] to drugs [22] . There are also some studies that PCT was extracted by liquid phase microextraction methods but different derivatization reactions were employed before the analyte extraction [23,24] …”