Ruiz Irene, Morales Ascensión, Barba Alberto, Oliva José
University of Murcia, Faculty of Chemistry, Department of Agricultural Chemistry, Geology and Pedology, Campus Espinardo, s/n, 30100 Murcia, Spain.
J AOAC Int. 2012 Jan-Feb;95(1):238-43. doi: 10.5740/jaoacint.10-407.
An analytical procedure was developed for the determination of some natural pesticides (piperonyl butoxide, nicotine, rotenone, spinosad, and abamectin B1a) in fruit matrixes. The quick, easy, cheap, effective, rugged, and safe (QuEChERS) method was used for extraction. Analysis of the extract was performed by LC-electrospray ionization (ESI)-MS/MS. The ions prominent in the ESI spectra were [M+Na]+ for abamectin B1a, [M+NH4]+ for piperonyl butoxide, and [M+H]+ for the rest of the compounds. A Zorbax SB-C18 column was used with a programmed gradient mobile phase consisting of (A) water containing 0.1% formic acid and 5 mM ammonium formate, and (B) acetonitrile containing 2 mM sodium acetate. The method was linear within the investigated concentration range, displaying a calibration curve correlation factor of 0.99. The CVs obtained were below 20%, and recoveries were in the 70-110% range.
建立了一种分析方法，用于测定水果基质中的某些天然农药（胡椒基丁醚、烟碱、鱼藤酮、多杀菌素和阿维菌素B1a）。采用快速、简便、廉价、高效、耐用且安全（QuEChERS）的方法进行提取。提取物通过液相色谱 - 电喷雾电离（ESI）- 串联质谱进行分析。在ESI光谱中，阿维菌素B1a的主要离子为[M + Na]+，胡椒基丁醚的主要离子为[M + NH4]+，其余化合物的主要离子为[M + H]+。使用Zorbax SB - C18柱，流动相采用程序梯度，由（A）含0.1%甲酸和5 mM甲酸铵的水，以及（B）含2 mM醋酸钠的乙腈组成。该方法在所研究的浓度范围内呈线性，校准曲线相关系数为0.99。所得变异系数低于20%，回收率在70 - 110%范围内。
