Method development, validation, and risk assessment of multiple pesticide residues of fruits in China

In this study, a muti-residue analysis method of 40 pesticides in five different categories of fruits in China was developed based on ultra-performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS). Five hundred real samples were analyzed and assessed for the dietary exposure risk. The sample treatment method was optimized by comparing four clean-up methods. The matrix effects of different fruits were evaluated. The analytical method was validated in terms of linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision. The results showed that the optimal method was the treatment by clean up with ODS (octadecylsilane) and MgSO₄. The matrix effect was the strongest in orange and weakest in apple. The LOD and LOQ of pesticides were 0.04–5.9 μg kg⁻¹ and 0.13–19.5 μg kg⁻¹, respectively. The recoveries at three spiked levels were ranged from 71.2 to 115.2% with the RSDs from 0.1 to 19.6%. Twenty-two pesticides were detected in 500 fruit samples from the major production regions of China, with concentrations ranging from 0.1 to 1930 μg kg⁻¹. A total of 13, 10, 9, 8, and 4 pesticides were detected in peach, orange, grape, apple, and strawberry. Both the acceptable daily intake (ADI) and acute reference dose (ARfD) for all the detected pesticides were lower than 100%, indicating that the dietary intake risks are acceptable and would not pose potential health risks.