She Yongxin, Wang Jing, Zheng Yongquan, Cao Weiqiang, Wang Rongyan, Dong Fengshou, Liu Xingang, Qian Mingrong, Zhang Hu, Wu Liqing
Institute of Quality Standards and Testing Technology for Agri-Products, Chinese Academy of Agricultural Science, 100081 Beijing, China; Institute of Veterinary and Animal Husbandry, Tibetan Academy of Agricultural and Animal Husbandry, 850009 Lhasa, China.
Institute of Quality Standards and Testing Technology for Agri-Products, Chinese Academy of Agricultural Science, 100081 Beijing, China.
Food Chem. 2012 May 1;132(1):502-7. doi: 10.1016/j.foodchem.2011.09.131. Epub 2011 Oct 10.
A method has been developed for the simultaneous determination of the concentration of nonylphenol (4-NP), nonylphenol monoethoxylates (NP1EO) and nonylphenol diethoxylates (NP2EO) in vegetables and crops by liquid chromatography-tandem quadrupole mass spectrometry (HPLC-MS/MS). These target compounds were extracted from vegetable and crop samples with acetonitrile, and then the extracts were cleaned using solid phase extraction with graphitised carbon black tandem primary secondary amine (PSA) cartridges. The MS method enabled highly reliable identification by monitoring the corresponding ammonium adduct M+NH4 in the positive mode for NP1EO and NP2EO, and the deprotonated molecule M-H in the negative mode for 4-NP. Recoveries for the spiked samples ranged from 65% to 118%. The limit of detection (LOD) of 4-NP, NP1EO and NP2EO was 3, 5 and 0.1μgkg(-1), respectively. This method would be useful for the quick and routine detection of the residues of 4-NP, NP1EO and NP2EO in vegetables and crops.
已开发出一种通过液相色谱 - 串联四极杆质谱法（HPLC - MS/MS）同时测定蔬菜和农作物中壬基酚（4 - NP）、壬基酚单乙氧基化物（NP1EO）和壬基酚二乙氧基化物（NP2EO）浓度的方法。这些目标化合物用乙腈从蔬菜和农作物样品中提取，然后提取物用石墨化炭黑串联伯仲胺（PSA）柱进行固相萃取净化。质谱方法通过在正模式下监测NP1EO和NP2EO的相应铵加合物M + NH4以及在负模式下监测4 - NP的去质子化分子M - H实现了高度可靠的鉴定。加标样品的回收率在65%至118%之间。4 - NP、NP1EO和NP2EO的检测限分别为3、5和0.1μgkg(-1)。该方法可用于快速、常规检测蔬菜和农作物中4 - NP、NP1EO和NP2EO的残留量。
