超高效液相色谱-串联质谱法快速测定纸质食品包装材料及容器中的7种双酚类化合物  

Rapid determination of 7 kinds of bisphenols by ultra-performance liquid chromatography-tandem mass spectrometry in paper food packaging materials and containers

作　　者：王军淋[1] 陆亚亚 张念华[1] 张晶[1] 张京顺[1] 蔡增轩[1] 

机构地区：[1]浙江省疾病预防控制中心,浙江杭州310051 [2]浙江中医药大学,浙江杭州310053

出　　处：《中国卫生检验杂志》2017年第13期1858-1862,共5页Chinese Journal of Health Laboratory Technology

摘　　要：目的建立超高效液相色谱-串联质谱法快速检测纸质食品包装材料和容器中的双酚A及其6种类似物。方法样品剪碎后经60%乙醇水溶液超声提取,提取液过滤后直接进超高效液相色谱-串联质谱分析。对7种双酚化合物的质谱断裂方式进行分析,优化了质谱参数、色谱分离条件及前处理条件(提取溶液、提取溶液体积、超声时间、超声温度)。结果 7种双酚类化合物浓度在2 ng/ml^150 ng/ml时,线性相关系数(r)≥0.997,方法检出限为0.003 mg/kg^0.03 mg/kg,定量限为0.01 mg/kg^0.10 mg/kg。在低(0.25 mg/kg)、中(1.00 mg/kg)、高(4.00 mg/kg)3个水平加标浓度下,7种双酚类化合物的回收率分别为77.82%~132.90%、85.48%~103.82%、93.04%~114.75%,相对标准偏差(RSD)分别为1.88%~6.43%、1.03%~3.81%、1.07%~4.80%。结论该方法简单、快速、准确、低毒,适合于纸质食品包装材料和容器中7种双酚类化合物的日常大批量筛查与确证。Objective To develop a method for the rapid determination of bisphenol A and its 6 analogues（ B,F,P,Z,AF,AP） in paper food packaging materials and containaers by ultra-performance liquid chromatography-tandem mass spectrometry（ UPLC-MS/MS）. Methods Firstly,the paper food packaging materials and the containers were sheared,and extracted by 60% ethanol aqueous solution with ultrasonic,then the extracted solution was analyzed by UPLC-MS/MS after filtration.The fracture mechanisms of 7 bisphenols in mass spectrum were anlyzed,then mass spectrum parameters,liqiud chromatography seperation and preparation conditions include extration solution,the ratio of volume of extration solution to sample mass,ultrsonic time and temperature were optimized. Results Good linearity was obtained when the concentrations of the 7 bisphenols were within 2 ng/ml-150 ng/ml,with correlation coefficient（ r） ≥ 0. 997. The limits of determination（ LOD） of 7 bisphenols were within 0. 003 mg/kg-0. 03 mg/kg and the limits of quantification（ LOQ） were within 0. 01 mg/kg-0. 10 mg/kg,respectively.The recoveries were within 77. 82%-132. 90%,85. 48%-103. 82%,93. 04%-114. 75%,and the RSDs were within1. 88%-6. 43%,1. 03%-3. 81%,1. 07%-4. 80% in 3 spiked levels（ 0. 25 mg/kg,1. 00 mg/kg,4. 00 mg/kg） of 7 bisphenols. Conclusion The established method is simple,rapid,accurate and of low toxin,which can be used for batches of samples＇ screening and confirmation of paper food packaging and containers materials.

关 键 词：双酚A 超高效液相色谱-串联质谱 纸质食品包装材料 纸质食品容器 

分 类 号：O657.63[理学—分析化学]