分散固相萃取-液相色谱-串联质谱法测定水基胶中的烷基酚聚氧乙烯醚  

Determination of alkylphenol ethoxylates in water-based adhesives by high performance liquid chromatography-tandem mass spectrometry combined with dispersive solid phase extraction

作　　者：杨飞[1] 孟冬玲[2] 邓惠敏[1] 纪元 贾楠[3] 王颖[1] 刘珊珊[1] 范子彦[1] 边照阳[1] 唐纲岭[1] YANG Fei;MENG Dongling;DENG Huimin;JI Yuan;JIA Nan;WANG Ying;LIU Shanshan;FAN Ziyan;BIAN Zhaoyang;TANG Gangling(China National Tobacco Quality Supervision&Test Center,Zhengzhou 450001,China;China Tobacco Guangxi Industrial Co.,Ltd.,Nanning 530001,China;Zhengzhou Tobacco Research Institute of CNTC,Zhengzhou 450001,China)

机构地区：[1]国家烟草质量监督检验中心,郑州市450001 [2]广西中烟工业有限责任公司,南宁市530001 [3]中国烟草总公司郑州烟草研究院,郑州市450001

出　　处：《烟草科技》2021年第10期54-62,共9页Tobacco Science & Technology

基　　金：国家烟草质量监督检验中心青年人才托举工程计划项目“雪茄烟叶发酵微生物组结构与菌株筛选”(562021CR0020)。

摘　　要：为实现水基胶中辛基酚聚氧乙烯醚(OPnEO)和壬基酚聚氧乙烯醚(NPnEO)的准确测定,建立了分散固相萃取结合液相色谱-串联质谱(HPLC-MS/MS)测定水基胶中OPnEO和NPnEO的分析方法。用甲醇提取样品,经C18分散固相萃取净化后,以Inspire HILIC为色谱柱,5 mmol/L醋酸铵溶液和乙腈为流动相进行梯度洗脱。在多反应监测模式(MRM)下进行MS/MS分析。结果表明:(1)在25 min内,不同聚合度的OPnEO和NPnEO均达到基线分离。(2)在3个不同添加浓度水平下(10、50、100 mg/kg),所有分析物的回收率在79.8%~93.8%之间,相对标准偏差(RSD)小于7.0%。所有化合物在给定的浓度范围内均有良好的线性关系(R2≥0.9987),检出限(LOD)和定量限(LOQ)范围分别为6.64~7.42和22.6~24.9μg/kg。(3)采用该方法对10个水基胶实际样品进行检测,仅在2个样品中检出NPnEO,所有样品中均未检出OPnEO。该方法稳定、准确且特异性强,可用于测定水基胶中OPnEO和NPnEO。To determine the alkylphenol ethoxylate levels in water-based adhesives accurately,a high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method combined with dispersive solid phase extraction to quantify octylphenol ethoxylate(OP_(n)EO)and nonylphenol ethoxylate(NP_(n)EO)in water-based adhesives was developed.Water-based adhesive samples were extracted with methanol,and then purified by C_(18) dispersive solid phase extraction.The extract solution was separated bygradient elution on an Inspire HILIC chromatographic column using 5 mmol/L ammonium acetate solution and acetonitrile as the mobile phases.MS/MS analysis was performed in multiple reaction monitoring mode(MRM).The results showed that:1)Baseline separation was realized for all OP_(n)EO and NP_(n)EO with different polymerization degrees within 25 minutes.2)Under optimized conditions,the spiked recoveries for all the analytes were in the range of 79.8%-93.8%with relative standard deviations(RSDs)less than 7.0%at the addition levels of 10,50 and 100 mg/kg.Good determination coefficients(R^(2)≥0.9987)were achieved for all the analytes in the given concentration ranges.The LODs and LOQs were in the range of 6.64-7.42 and22.6-24.9μg/kg respectively.3)Ten actual water-based adhesive samples were tested with the developed method.NP_(n)EO was detected only in 2 samples and OP_(n)EO was not detected in all the samples.This method is stable and accurate with strong specificity,and can be used to determine the OP_(n)EO and NP_(n)EO in water-based adhesives.

关 键 词：辛基酚聚氧乙烯醚 壬基酚聚氧乙烯醚 水基胶 高效液相色谱-串联质谱 分散固相萃取 

分 类 号：O657[理学—分析化学] O652.6[理学—化学]