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采用分散固相萃取和液相色谱-串联质谱法同时测定蔬菜和水果中的16种酰胺类杀菌剂

Simultaneous determination of sixteen amide fungicides in vegetables and fruits by dispersive solid phase extraction and liquid chromatography-tandem mass spectrometry.

作者信息

Wu Yin-Liang, Chen Ruo-Xia, Zhu Yong, Zhao Jian, Yang Ting

机构信息

Ningbo Academy of Agricultural Science, Ningbo 315040, PR China; Laboratory of Quality and Safety Risk Assessment for Agricultural Products (Ningbo), Ministry of Agriculture, Ningbo 315040, PR China.

Ningbo Academy of Agricultural Science, Ningbo 315040, PR China; Laboratory of Quality and Safety Risk Assessment for Agricultural Products (Ningbo), Ministry of Agriculture, Ningbo 315040, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2015 May 1;989:11-20. doi: 10.1016/j.jchromb.2015.02.038. Epub 2015 Mar 7.

Abstract

A modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method using multi-walled carbon nanotubes (MWCNTs) as a reversed-dispersive solid phase extraction (r-dSPE) material combined with ultra-high liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was developed for the simultaneous determination of 16 novel amide fungicides in vegetables and fruits. After extraction with acetonitrile, a dSPE cleanup procedure, which was developed after the optimization of the type and amount of MWCNTs, the pH value of the extract, the extraction time for MWCNTs, and the type of eluent with MWCNTs material, was conducted. The determination of the target compounds was conducted in less than 7.0 min while the specificity is ensured through the MRM acquisition mode. The linearity of the analytical response across the studied range of concentrations (0.25-500 μg/L) was excellent, obtaining correlation coefficients higher than 0.997. The samples were quantified with the matrix matched standard solutions. The average recoveries in cabbage, celery, strawberry, and grape at three spiked levels (0.01, 0.5, and 5.0mg/kg) were ranged from 72.4 to 98.5% with all RSDs lower than 10%. The limits of detection were below 0.003 mg/kg and the limits of quantification did not exceed 0.01 mg/kg in all matrices. The method demonstrated to be suitable for the simultaneous determination of 16 novel amide fungicides in vegetables and fruits.

摘要

建立了一种改进的快速、简便、廉价、高效、耐用且安全的(QuEChERS)方法,该方法使用多壁碳纳米管(MWCNTs)作为反相分散固相萃取(r-dSPE)材料,并结合超高效液相色谱串联质谱(UHPLC-MS/MS),用于同时测定蔬菜和水果中的16种新型酰胺类杀菌剂。用乙腈提取后,在优化了MWCNTs的类型和用量、提取物的pH值、MWCNTs的提取时间以及与MWCNTs材料一起使用的洗脱剂类型后,进行了分散固相萃取净化程序。目标化合物的测定在不到7.0分钟内完成,同时通过多反应监测(MRM)采集模式确保了特异性。在所研究的浓度范围(0.25 - 500μg/L)内,分析响应的线性良好,相关系数高于0.997。样品用基质匹配标准溶液进行定量。在三种加标水平(0.01、0.5和5.0mg/kg)下,卷心菜、芹菜、草莓和葡萄中的平均回收率在72.4%至98.5%之间,所有相对标准偏差(RSD)均低于10%。所有基质中的检测限均低于0.003mg/kg,定量限均不超过0.01mg/kg。该方法证明适用于同时测定蔬菜和水果中的16种新型酰胺类杀菌剂。

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