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JA0018 Multiresidue Analysis of 58 Pesticides in Bean Products by Disposable Pipet Extraction (DPX) Cleanup and Gas Chromatography−Mass Spectrometry Determination
来源:Journal Of Agricultural and Food Chemistry | 作者:Ziang Li | 发布时间: 2149天前 | 3014 次浏览 | 分享到:
A method based on disposable pipet extraction (DPX) sample cleanup and gas chromatography with mass spectrometric detection by selected ion monitoring (GC/MS-SIM) was established for 58 targeted pesticide residues in soybean, mung bean, adzuki bean and black bean. Samples were extracted with acetonitrile and concentrated (nitrogen gas flow) prior to being aspirated into DPX tubes. Cleanup procedure was achieved in a simple DPX-Qg tube. Matrix-matched calibrations were analyzed, and the limits of quantification (LOQ) of this method ranged from 0.01 mg kg−1 to 0.1 mg kg−1 for all target compounds. Coefficients of determination of the linear ranges were between 0.9919 and 0.9998. Recoveries of fortified level 0.02 mg kg−1 on soybean, mung bean, adzuki bean and black bean were 70.2−109.6%, 69.1−119.0%, 69.1−119.8%, and 69.0−120.8%, respectively, for all studied pesticides. Moreover, pesticide risk assessment for all the detected residues in 178 market samples at Beijing market area was conducted. A maximum 0.958% of ADI (acceptable daily intake) for NESDI (national estimated daily intake) and 55.1% of ARfD (acute reference dose) for NESTI (national estimated short-term intake) indicated low diet risk of these products.
1 Introduction

Bean products are one of the fundamental foods recommended by the health food pyramid. Acting as both grains and vegetables in prevention of cancer, they are rich in protein and vitamins but low in calories.1 However, public concern over food safety, especially the potential health risk to humans cause by the high levels of pesticide residues, has increased. Measuring the trace levels of pesticide residue in beans by a simple, reliable and environmentally friendly method is becoming important. It is a particularly challenging task to test routinely and comprehensively the multiresidue pesticides in large amounts of sample matrix components that may cause false positive results. In order to clean these components up, conventional liquid−liquid extraction (LLE) is time-consuming and laborious and usually involves significant glassware usage and disposal of large volumes of hazardous organic waste.2 Therefore, solid phase extraction (SPE) techniques are worth considering because of their selectivity, capability to preconcentrate pesticide, high efficiency of using organic solvents and variety of the adsorbent materials in the SPE column.3,4 Furthermore, prior to chromatographic analysis, SPE cartridges have extended the application of SPE techniques for extracting and concentrating pesticides in a broad range of sample matrices.5−7 However, SFE often requires separate optimization for different analyte types and may not extract different classes of pesticides in foods with the same efficiency.8 Besides LLE and SPE, there are some new approaches, such as solid phase microextraction (SPME), matrix solid phase dispersion (MSPD) and stir-bar sorptive extraction (SBSE) also available to match some aspects of the requirement. But by considering their imperfections of expensiveness and fragileness,1 large requirement of adsorbent and solvent9,10 or commercial availability and good recoveries for polar pesticides,1,3,11 they are probably not able to match all of our purposes. The QuEChERS method (quick, easy, cheap, effective, rugged, and safe) has recently attracted attention for pesticide analysis.12−14 Its main advantage is comprehensiveness, being useful for the analysis of pesticides of varying polarities, by virtue of the fact that the sorbent removes fatty acid components and pigments from acetonitrile extracts without interacting with the target analytes. Much of the literature with QuEChERS suggests that better results are obtained using the dispersive procedure, where mixing with the loose sorbent provides efficient removal of matrix compounds and provides higher recoveries of pesticides with minimal solvent.1