| 固相萃取-超高效液相色谱-串联质谱法测定美国进口水果中15种高风险农药及助剂残留 |
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| 引用本文： | 兰丰,李晓亮,段小娜,姜蔚,臧宏伟,刘传德,周先学,鹿泽启,王志新,华则科,王添翼.固相萃取-超高效液相色谱-串联质谱法测定美国进口水果中15种高风险农药及助剂残留[J].农药学学报,2019,21(4):475-482. |
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| 作者姓名： | 兰丰 李晓亮 段小娜 姜蔚 臧宏伟 刘传德 周先学 鹿泽启 王志新 华则科 王添翼 |
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| 作者单位： | 1.山东省烟台市农业科学研究院/农业农村部果品质量安全风险评估实验室 (烟台)，山东 烟台 265500 |
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| 基金项目： | 国家农产品质量安全风险评估项目（GJFP2019011）；山东省农业科学院农业科技创新工程：山东省主要农产品质量安全风险评估与控制技术研究（GXGC2016B17） |
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| 摘 要： | 建立了固相萃取-超高效液相色谱-串联质谱 (SPE-UPLC-MS/MS) 测定美国进口水果中15种高风险农药及助剂（乙酰甲胺磷、灭多威、噻虫嗪、噻菌、啶虫脒、西玛津、嘧霉胺、咯菌腈、啶酰菌胺、甲氧虫酰肼、腈菌唑、环酰菌胺、四氟醚唑、增效醚、毒死蜱）残留量的分析方法。样品经破壁机匀浆，乙腈涡旋提取，氨基固相萃取柱净化，岛津Shim-pack XR-ODS色谱柱分离 (75 mm × 2.0 mm，1.6 μm)。采用电喷雾离子源多反应监测模式进行质谱检测，外标法定量。在0.001~0.5 mg/L范围内，15种农药及助剂的质量浓度与对应的峰面积间线性关系良好，R2 ≥ 0.999 5。以梨、葡萄和苹果3种基质为例验证了方法的准确度和精密度。结果表明:在0.005~0.5 mg/kg添加水平下，15种农药及助剂的平均回收率在80%~115%之间，相对标准偏差在5.5%~16%之间，定量限为0.005~0.01 mg/kg。该方法简便、快速、可靠，适用于同时测定水果中上述15种农药及助剂残留。
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| 关 键 词： | 固相萃取 超高效液相色谱-串联质谱 进口水果 高风险农药 助剂 最大残留限量 |
| 收稿时间： | 2019/2/14 0:00:00 |
Determination of 15 high-risk pesticide and adjuvant residues in fruits from USA by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry |
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| LAN Feng,LI Xiaoliang,DUAN Xiaon,JIANG Wei,ZANG Hongwei,LIU Chuande,ZHOU Xianxue,LU Zeqi,WANG Zhixin,HUA Zeke and WANG Tianyi.Determination of 15 high-risk pesticide and adjuvant residues in fruits from USA by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2019,21(4):475-482. |
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| Authors: | LAN Feng LI Xiaoliang DUAN Xiaon JIANG Wei ZANG Hongwei LIU Chuande ZHOU Xianxue LU Zeqi WANG Zhixin HUA Zeke and WANG Tianyi |
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| Institution: | 1.Laboratory of Quality and Safety Risk Assessment for Fruit (Yantai), Ministry of Agriculture and Rural Affairs, Yantai Academy of Agricultural Sciences in Shandong Province, Yantai 265500, Shandong Province, China2.Agricultural Technology Promotion Center of Laiyang, Laiyang 265200, Shandong Province, China |
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| Abstract: | A method was developed for the quantative determination of 15 high-risk pesticide and adjuvant (acephate, methomyl, thiamethoxam, thiabendazole, acetamiprid,simazine, pyrimethanil, fludioxonil, boscalid, methoxyfenozide, myclobutanil, fenhexamid, tetraconazole, piperonyl butoxide, chlorpyrifos) residues by SPE-ultra performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The samples were homogenized, extracted with acetonitrile, and cleaned-up by amino solid phase extraction column. The separation was performed on a Shimadu Shim-pack XR-ODS column (75 mm × 2.0 mm, 1.6 μm). The compounds were identified by MS/MS and multiple reaction monitoring (MRM) mode, and quantified by external standard method. The linearities of 15 pesticides and adjuvants were in the concentration range of 0.001-0.5 mg/L, with the correlation coeffecients higher than 0.999 5. At the fortified levels from 0.005 mg/kg to 0.5 mg/kg in pear, grape and apple, the average recoveries of all 15 pesticides and adjuvants ranged from 80% to 115% with the relative standard deviations varied from 5.5% to 16%. The limits of quantification (LOQs) of the analytes were ranged from 0.005 to 0.01 mg/kg. This method is simple, rapid, accutate and therefore, suitable for the confirmation and quantification of the 15 pesticides and adjuvants in fruits. |
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| Keywords: | solid phase extraction ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) imported fruits high-risk pesticides adjuvant maximum residue limit (MRL) |
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