环境内分泌干扰物辛基酚、壬基酚及短链壬基酚聚氧乙烯醚残留同步检测方法  

Simultaneous Determination of Octylphenol, Nonylphenol and Short Chain Nonylphenol Ethoxylate in AgroProducts and Food Packages by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：杨锚[1,2] 王淼[1,3] 佘永新[1,3] 李腾飞[1,3] 王静[1,3] 王珊珊[1,3] 金芬[1,3] 金茂俊[1,3] 邵华[1,3] 曹维强[4] 

机构地区：[1]中国农业科学院农业质量标准与检测技术研究所,北京100081 [2]农业部农药检定所,北京100084 [3]农业部农产品质量标准研究中心,北京100081 [4]广东惠州出入境检验检疫局检测中心,广东惠州516000

出　　处：《农业环境科学学报》2014年第7期1460-1464,共5页Journal of Agro-Environment Science

基　　金：国家科技支撑计划(2011BAK10B05-05);国家自然科学基金(31260620);科技基础性工作专项(2013FY110100)

摘　　要：建立了环境内分泌干扰物辛基酚、壬基酚及短链壬基酚聚氧乙烯醚降解产物的高效液相色谱串联质谱分析方法。选择易受环境污染的玉米、白菜等农产品及目标物可能迁移到环境中的食品包装材料为研究对象，经过液液萃取、浓缩，乙腈甲苯（3：1）溶液溶解，经ENVITMCarblI／PSA氨基固相萃取柱净化，甲醇一二氯甲烷（4：3）溶液为洗脱液。采用Agilent ZORBAX RX-C18柱，以甲醇：10mmol·L^-1乙酸铵（9：1）为流动相，梯度洗脱分离后，在LC—MS／MS多反应监测模式下正负离子同时扫描进行定性与定量分析。结果表明，该方法对辛基酚、壬基酚、壬基酚一氧乙烯醚和壬基酚二氧乙烯醚的检出限分别为O．03、0.6、1．6、0．03μg·kg^-1，在不同基质中添加浓度为0．5-5μg·kg^-1的四种物质平均回收率在62％～113％之间。对实际样品进行检测时，在蔬菜和粮食作物及其包装材料中分别检测到不同含量的上述物质，表明该方法准确、快速、灵敏度高，可用于农产品和食品包装材料中该类物质的监控。A novel method was established for simultaneous determination of octylpehenol （OP）, nonylphenol （NP）, nonylphenol mo- noethoxylates（NPEO1 ） and nonylphenol diethoxylates （NPEO2） in agro-products and food packages with liquid chromatography-tandem quadrupole mass spectrometry（ HPLC-MS/MS ）. These analytes were extracted from vegetables, crops and food packaging materials with acetonitrile and toluene solution. The extracts were cleaned using solid phase extraction with graphitized carbon black tandem and primary secondary amine（PSA） cartridges. LC-MS/MS was utilized for simultaneous analysis of OP, NP, NPEO1 and NPEO2. After chromatograph- ic separation on Agilent ZORBAX RX-C 18 column with methanol-10 mmol· L-1ammonium acetate gradient elution, qualitative and quanti- tative analyses were carried out under the simultaneous scanning models of positive and negative. The average recoveries for agro-products and food packaging materials at spiked levels of 0.5-5 μg·kg^-1 were from 62% to 113%. The limit of detection （LOD） of OP, NP, NPEO 1 and NPEO2 was 0.03 μg·kg^-1, 0.6 μg·kg^-1, 1.6 μg·kg^-1 and 0.03 μg·kg^-1, respectively. This method is accurate, rapid, and sensitive, and could be used for quick and routine determination of OP, NP, NPEO1 and NPEO2 in agro-products and food packages.

关 键 词：辛基酚 壬基酚 短链壬基酚聚氧乙烯醚类 高效液相色谱串联质谱法 

分 类 号：X830.2[环境科学与工程—环境工程]