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| Analysis of 297 Pesticides Residues in Peanut by Gas Chromatography－Tandem Mass Spectrometry with Automatic QuEChERSAnalysis of 297 Pesticides Residues in Peanut by Gas Chromatography－Tandem Mass Spectrometry with Automatic QuEChERS |
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| DOI： |
| KeyWord:peanut multiresidue analysis automatic QuEChERS gas chromatography－tandem mass spectrometry（GC－MS/MS） |
| Author | Institution |
| JIANG Kang-li，HU Bin，WU Xing-qiang，XIE Yujie，LI Tie-mei，FAN Chun-lin，WANG Ming-lin，WANG Wen-wen，CHEN Hui |
1. Chinese Academy of Inspection and Quarantine，Beijing ，China;2. College of Food Science and Engineering，Shandong Agricultural University，Taian ，China;3. Agilent Technologies （China）Limited，Beijing ，China） |
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| Abstract: |
| Peanut is an important oil and economic crop in China， which has been well accepted by consumers as it could be eaten fresh， used to extract oil， and also be processed into peanut products. In recent years， as a result of abuse of pesticide， the quality and safety risks of peanuts have become an increasingly important issue. Gas chromatography－tandem mass spectrometry（GC－MS/MS） combined with automatic QuEChERS pre-treatment equipment is an effective method for the detection of multi-pesticide residues. Thus， a rapid method based on GC－MS/MS was established for the simultaneous determination of 297 pesticides in peanut. The pretreatment parameters was optimized by comparing the spiked recoveries obtained from different extract solvents（acetonitrile， acetonitrile containing 1% acetic acid and acetonitrile containing 2% acetic acid）， different volumes of extract solvents（10， 15 and 20 mL）， different buffer salts（anhydrous magnesium sulfate， sodium acetate） and different purification combinations（primary secondary amine（PSA） + octadecylsilane（C18）， PSA + C18-bonded zirconium rubber（Z－Sep+）， PSA + C18 + Z－Sep+， EMR－lipid）. Under the optimized conditions， 2 g samples were soaked with 2 mL ultrapure water， the pesticides in the peanuts were extracted using acetonitrile containing 1% acetic acid， salted out using 4 g anhydrous magnesium sulfate and 1 g sodium acetate. Then the solution was purified using 100 mg PSA + 200 mg C18 + 100 mg Z－Sep + automatic QuEChERS pre-treatment device combined with centrifuge device by vortex vibration through a purification tube which included an inner tube， an outer tube and a filtration membrane. Pesticides were separated on an HP－5MS UI capillary column using temperature programming， determined by GC－MS/MS in positive ion multiple mode and quantified by external standard method. The matrix effects were evaluated with the established method. Results showed that 25.25% of the pesticides exhibited enhancing matrix effects， while 2.02% of them exhibited inhibition matrix effects and 72.73% of them exhibited weak matrix effects. Matrix-matched standard curve was used to reduce the matrix effects on detection of the pesticide residues. Methodological verifications were evaluated for the established method， and the results showed that there were good linear relationships for all the pesticides in the corresponding range， with their correlation coefficients（r2） greater than 0.995. The limits of quantitation（LOQs） were 2－10 μg/kg. The recoveries for 297 pesticides at four spiked levels of 10， 20， 50 and 100 μg/kg were in the range of 72.7%－116%， 71.9%－117%， 73.2%－112% and 71.5%－120%， with relative standard deviations（RSDs） of 0.90%－15%， 0.70%－15%， 0.60%－14% and 0.40%－15%， respectively. The proposed method was applied to the detection of 8 batches of peanut samples purchased from local supermarket. The results demonstrated that 6 batches of the peanut samples were found containing pesticide residues， in which 17 pesticides were detected in total. The concentration of dicrotophos was the highest among all pesticides， reaching 34.67 μg/kg. Therefore， the developed method was simple， rapid， sensitive and automatic， and was suitable for the rapid detection of pesticide residues in peanuts. |
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