建立了QuEChERS-液相色谱-串联质谱同时测定棕榈原油中敌草快、乐果、倍硫磷、倍硫磷亚砜、倍硫磷砜、氟吡甲禾灵残留量的方法。以回收率及基质效应为考察指标,评估了乙二胺-N-丙基硅烷(PSA)/C18混合物、C18键合锆胶(Z-Sep+)/C18混合物、Z-Sep+、C18 4种分散吸附剂的净化效果,结果表明Z-Sep+/C18的净化效果最佳。样品采用含1%(v/v)乙酸的甲醇溶液提取,Z-Sep+/C18分散固相萃取净化;液相色谱以Atlantis T3色谱柱梯度洗脱分离,质谱分析采用电喷雾正离子电离、多反应监测模式,以基质匹配校准曲线外标法进行定量。6种农药在3个添加水平(10、20、250 μg/kg)下的回收率范围为70.0%~97.9%,相对标准偏差范围为2.6%~10.2%; 6种农药的定量限(S/N≥10)为0.1~2.5 μg/kg。该方法简便、灵敏、准确、环保,适用于棕榈原油中上述6种农药残留的定性、定量分析。
A fast method based on QuEChERS methodology was developed for the simultaneous determination of diquat, dimethoate, fenthion, fenthion-sulfoxide, fenthion-sulfone, haloxyfop-methyl in crude palm oil using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The clean-up effects of four dispersive sorbents were evaluated in terms of recoveries and matrix effects. The four sorbents were the mixture of primary secondary amine (PSA) and C18, a mixture of two sorbents a bonded C18 zirconia-coated silica (Z-Sep+) and C18, Z-Sep+, C18. As a result, the best effects were obtained from using the mixture of Z-Sep+ and C18 sorbents. The samples were extracted with methanol containing 1%(v/v) acetic acid. The extracts were cleaned up with dispersive solid phase extraction using Z-Sep+/C18 sorbents. Chromatographic analysis was carried out on an Atlantis T3 column with gradient elution. The pesticides were analyzed by positive electrospray ionization-tandem mass spectrometry under multiple reaction monitoring mode. The quantification was achieved using matrix-matched standard calibrations as external standard. The recoveries at the fortification levels of 10, 20 and 250 μg/kg in crude palm oil ranged from 70.0% to 97.9% with the relative standard deviations of 2.6%-10.2%. The limits of quantification (S/N≥10) were 0.1-2.5 μg/kg. The method has been proven to be simple, sensitive, accurate and environmental and thus suitable for the determination of the six pesticide residues above in crude palm oil.
参考文献
| [1] | GB 2763-2014 |
| [2] | Zhuang W J. The Global Regulations on Maximum Residue Limits (MRLs) for Pesticides in Foodstuffs and Feedstuffs (Volume Ⅰ-Ⅱ). Beijing:Chemical Industry Press, 2010 庄无忌. 国际食品饲料中农药残留限量法规(Ⅰ-Ⅱ卷). 北京:化学工业出版社, 2010 |
| [3] | Sack C, Smoker M, Chamkasem N, et al. J Agric Food Chem, 2011, 59:6383 |
| [4] | GB/T 20770-2008 |
| [5] | Xu J, Wang L, Huang H J, et al. Chinese Journal of Chromatography, 2015, 33(3):242 徐娟, 王岚, 黄华军, 等. 色谱, 2015, 33(3):242 |
| [6] | GB/T 5009.221-2008 |
| [7] | Chen J, Liu Z J, An B C, et al.. Chinese Journal of Chromatography, 2012, 30(10):1068 陈静, 刘召金, 安保超, 等.. 色谱, 2012, 30(10):1068 |
| [8] | SN/T 0293-2014 |
| [9] | Li J, Yang F, Lu S Y, et al. Chinese Journal of Analysis Laboratory, 2014, 33(5):537 李捷, 杨方, 卢声宇, 等. 分析试验室, 2014, 33(5):537 |
| [10] | Hao C Y, Zhao X M, Morse D, et al. J Chromatogr A, 2013, 1304:169 |
| [11] | Kolberg D I S, Mack D, Anastassiades M, et al. Anal Bioanal Chem, 2012, 404:2465 |
| [12] | Moreno-González D, Huertas-Pérez J F, García-Campaña A M, et al. Talanta, 2014, 128:299 |
| [13] | Sapozhnikova Y, Lehotay S J. Anal Chim Acta, 2013, 758:80 |
| [14] | Rajski L, Lozano A, Uclés A, et al. J Chromatogr A, 2013, 1304:109 |
| [15] | Lozano A, Rajski L, Uclés S, et al. Talanta, 2014, 118:68 |
| [16] | Wang L Z, Huang X Y, Wang D F, et al. Chinese Journal of Chromatography, 2015, 33(5):501 王连珠, 黄小燕, 王登飞, 等. 色谱, 2015, 33(5):501 |
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