采用 QuEChERS-超高效液相色谱-串联质谱技术，建立了蔬菜中常见的隐性农药、禁限用农药、植物生长调节剂等检出率较高的41种农药残留的测定方法。蔬菜样品用1％（ v／v）乙酸-乙腈溶液提取，乙二胺-N-丙基硅烷（ PSA）净化后直接进样分析，采用正、负离子多反应监测（ MRM ）模式，外标法定量。结果表明，在优化后的QuEChERS、色谱和质谱条件下，41种农药在1.0~100μg／L范围内线性关系良好，相关系数（ r2）大于0.999，检出限为0.003~1.00μg／kg，不同基质中的平均回收率范围为74.1％~120.4％，相对标准偏差（ RSD）范围为2.8％~11.9％。该方法快速简便、灵敏度高、净化效果好，可用于蔬菜中41种农药的快速测定，为蔬菜质量安全风险评估工作提供了有力保障。
A multiresidue analytical method for the rapid determination of 41 pesticide residues in vegetables was developed by using QuEChERS-ultra performance liquid chromatography-tan-dem mass spectrometry( UPLC-MS/MS),including recessive pesticides,banned pesticides and pesticides with restrict use,plant growth regulators and some other pesticides with high detec-tion rates. The vegetable sample was extracted by 1%( v/v)acetic acid-acetonitrile,cleaned-up by primary secondary amine( PSA)and injected for analysis. The positive and negative ion modes and multiple reaction monitoring( MRM)mode were used in the analysis,and the ana-lytes were quantified by the external standard method. Under the conditions of optimized QuEChERS,chromatography and mass spectrometry,the 41 pesticides showed good linearities in the range of 1. 0 μg/L to 100 μg/L,with the correlation coefficients(r2)higher than 0. 999. The limits of detection of the method were 0. 003 μg/kg to 1. 00 μg/kg. The average recoveries of the 41 pesticides in different matrices were in the range of 74. 1%—120. 4% with the relative standard deviations from 2. 8% to 11. 9%. The method has the advantages of rapidity,simplici-ty,high sensitivity and better purification effect. It is suitable for the rapid determination of the common pesticides in vegetables,and it provides a strong guarantee for the risk assessment of the quality and safety of vegetables.
参考文献
| [1] | Chen C;Qian Y;Chen Q.[J].FOOD CONTROL,201122(7):1114. |
| [2] | Naik S;Prasad R.[J].J Chem Health Saf,200613(6):12. |
| [3] | 胡业琴;郗存显;曹淑瑞;王国民;李贤良;张雷;张云怀.介孔氧化铝净化-气相色谱法同时测定蔬菜、水果及茶叶中16种有机磷农药残留[J].色谱,2014(7):784-788. |
| [4] | Colume A;Cardenas S;Gallego M.[J].Analytica Chimica Acta,2001436(1):153. |
| [5] | 侯如燕;卞红正;赵秀霞;胡祎芳;苏婷;王孝辉;宛晓春.固相萃取-液相色谱测定复杂基质蔬菜中9种烟碱类残留[J].分析测试学报,2011(1):58-63. |
| [6] | Melo A;Aguiar A;Mansilha C.[J].Food Chemistry,2012130(4):1090. |
| [7] | 郭春景;李娜;王建忠.超高效液相色谱-串联质谱法快速测定8种蔬菜中114种农药残留[J].质谱学报,2014(3):279-288. |
| [8] | 柳菡;徐锦忠;丁涛;张晓燕;杨雯筌;赵增运;陈惠兰;吴斌;沈崇钰;蒋原.蔬菜中26种农药残留的高效液相色谱-串联质谱法测定[J].分析测试学报,2009(2):181-185. |
| [9] | 葛娜;刘晓茂;李学民.[J].分析测试学报,201230(12):1351. |
| [10] | 陈红平;刘新;汪庆华;蒋迎.气相色谱-串联质谱检测水果、蔬菜中抗蚜威、甲霜灵和克螨特残留量[J].质谱学报,2010(4):220-223. |
| [11] | 黄何何;张缙;徐敦明;周昱;罗佳;吕美玲;陈树宾;王连珠.QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J].色谱,2014(7):707-716. |
| [12] | 王菲;李彤;马辰.超高效液相色谱-串联质谱法测定中药材中三唑类杀菌剂及三嗪类除草剂的残留量[J].色谱,2013(3):191-199. |
| [13] | Zhao H H;Xu J;Dong F S.[J].Anal Methods,20146(12):4336. |
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