| 高效液相色谱-串联质谱法测定板栗中58种农药残留 |
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| 引用本文： | 侯霞,赵雁冰,麻兵继,杨红,查丽娟.高效液相色谱-串联质谱法测定板栗中58种农药残留[J].河北农业科学,2016(6):97-105. |
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| 作者姓名： | 侯霞 赵雁冰 麻兵继 杨红 查丽娟 |
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| 作者单位： | 1. 唐山出入境检验检疫局,河北 唐山,063000;2. 河南农业大学,河南 郑州,450002 |
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| 基金项目： | 河南省基础与前沿技术研究项目(1423004132081) |
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| 摘 要： | 为建立适用于板栗多种农药残留检测的高效液相色谱-串联质谱(HPLC-MS/MS)分析方法,以乙腈为提取溶剂,样品经高速均质提取,PSA、C18固相萃取柱净化后用HPLC分离,以Agilent C18(2.7μm,2.1 mm×100 mm)为色谱柱,甲醇和0.1%甲酸-2 mmol/L乙酸铵水为流动相进行梯度洗脱,柱温30℃,进样量5.0μL、流速300μL/min,在ESI离子源、正离子扫描、动态MRM模式下,以保留时间和质荷比对分离的组分定性,外标法峰面积定量。结果表明:58种农药在各自的线性范围内相关性良好(r0.99),各农药的加标回收率范围为60%~120%,符合残留检测要求。
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| 关 键 词： | 高效液相色谱-串联质谱 (HPLC-MS/MS) 板栗 农药残留 |
Determination of 58 Pesticides in Chinese Chestnut Using High Performance Liquid Chromatography-tandem Mass Spectrometry |
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| Abstract: | A method for the determination of 58 pesticides in Chinese chestnut was developed by using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) . The sample was extracted by acetonitrile in high-speed homogenization,cleaned by PSA,C18 Solid Phase Extraction Column and separated by HPLC. Chromatographic separation was performed on Agilent C18 column (2.7μm,2.1 mmí100 mm) using a gradient elution of methanol and 0.1% formic acid-2 mmol/L ammonium acetate as mobile phases,at a flow rate of 300 μL/min. The column temperature was 30 ℃ and the sample size was 5.0 μL. The peaks were de-tected by an electrospray ionization tandem mass spectrometry with dynamic MRM. Pesticide qualitation was based on the retention time and mass charge ratio and its quantitation was based on the peak area of fragment ion. The results indicated that the calibration curve of 58 pesticides was in good linear (r>0.99),and the aver-age recovery of main peaks were in the range of 60%-120%. As a result, this method is simple, fast and credible and can be applied to screen and detect these pesticide residues in Chinese chestnut. |
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| Keywords: | High performance liquid chromatography-tandem mass spectrometry (HPLC-MS /MS) Chinese chestnut Pesticide residue |
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