A novel approach for simultaneous analysis of perchlorate (ClO4−) and bromate (BrO3−) in fruits and vegetables using modified QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry

Abstract

Perchlorate (ClO) and bromate (BrO) are mainly determined by ion chromatography methods. The present work aims to develop a modified QuEChERS combined with ultrahigh performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for simultaneous analysis of ClO and BrO in fruits and vegetables including cherry tomato, strawberry, tomato, potato, lettuce and pakchoi. Two target inorganic anions were separated on a Diamonsil C18(2) column by gradient elution, scanned in ESI negative mode and detected under multiple reactions monitoring (MRM). Limit of detection (LOD) and method limit of quantification (MLOQ), matrix effect, accuracy and precision of the developed method were investigated. Results were linear in their concentration ranges, with coefficients of determination (r) bigger than 0.999. LODs for ClO and BrO were 0.1 μg/L and 0.5 μg/L, respectively. The validated method provided sufficient selectivity, sensitivity and accuracy to screen for ClO and BrO with ignorable matrix effects. Recoveries for different kinds of negative samples at 3 spiked levels were between 82.0% and 99.5%. Both intraday-precision and interday-precision were satisfactory, showing RSDr values in the range of 2.1-7.1% and RSD values in the range of 7.2-10.8%. The proposed method was successfully applied to determine target inorganic anions in several fruits and vegetables. Perchlorate was detected in 12 vegetable samples with the concentrations ranged from 21 μg/kg to 162 μg/kg. Results indicated that there was wide ClO contamination in vegetables, confirming its urgency for monitoring harmful inorganic anions in our daily consumed vegetables.

Comparison of Two Methods for the Determination of Selected Pesticides in Honey and Honeybee Samples

“…However, for several years, the basic QuEChERS procedure has been modified many times and used for determination of pesticide residues in honey [ 11 , 12 ], wax [ 13 , 14 ], pollen [ 15 ], honeybees [ 16 , 17 , 18 ], royal jelly [ 19 , 20 ], bumblebees [ 21 , 22 ] and beebread [ 23 , 24 , 25 ], coupled with analysis using LC-MS/MS and GC-MS/MS. Modified QuEChERS has also been used in the analysis of perchlorate (ClO 4− ) and bromate (BrO 3− ), biogenic amines, and quaternary ammonium compounds in various kinds of food matrix [ 26 , 27 ].…”

A high‐throughput screening method for determination of multi‐antibiotics in animal feed

“…Method matrix effect for each analyte in UHPLC‐MS/MS analysis may result from various physical and chemical processes and it is difficult to eliminate . The matrix effect was investigated by comparing the slope of matrix matched calibration curves with pure solvent working curves.…”

Rapid determination of hexavalent chromium in textiles by a novel ammonium pyrrolidine dithiocarbamate derivatization combined with UHPLC–MS/MS

“…In the meantime, the MEs were calculated according to the slopes’ ratio of calibration curve of the matrix versus standard working curve of pure solvent (ME > 1 and ME < 1 represent matrix enhancement and matrix suppression, respectively) . The LOD and LOQ were calculated at S/N = 3 and 10, respectively . The LOD and LOQ of the instrument were calculated by measuring the standard solution with low concentration, while the LOD and LOQ of the method were determined by the low level of Cr(VI) spiked experiment and dilution factor (400 times) in sample pretreatment.…”