高效液相色谱-串联质谱法测定玩具中双酚A的迁移量  

Determination of Migration of Bisphenol A in Toys by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李函珂 张青[1] 黄宁珊 周懿琦 林捷聪 林绍鹏[1] 田勇[1] 蚁乐洲[1] 刘崇华[1] 黄理纳[1] LI Han-ke;ZHANG Qing;HUANG Ning-shan;ZHOU Yi-qi;LIN Jie-cong;LIN Shao-peng;TIAN Yong;YI Le-zhou;LIU Chong-hua;HUANG Li-na(Guangdong Inspection and Quarantine Technology Centre,Guangzhou 510623,China)

机构地区：[1]广东检验检疫技术中心,广东广州510623

出　　处：《分析测试学报》2018年第10期1244-1250,共7页Journal of Instrumental Analysis

基　　金：国家重点研发计划课题(2016YFF0203705);广东省科技计划项目(2014A04041066);国家标准项目资助(20161303-T-607)

摘　　要：建立了测定玩具中双酚A迁移量的高效液相色谱-串联质谱(HPLC-MS/MS)方法。改进了欧盟玩具安全标准EN 71-10:2005以水为模拟液的迁移条件,提出了迁移后模拟液经混合纤维素酯(MCE)过滤器过滤后直接由HPLC-MS/MS分析的方法。研究了不同材质针式过滤器对双酚A的影响。结果表明,聚酰胺(PA、尼龙66)和聚醚砜(PES)过滤器会导致双酚A大量损失,而MCE过滤器对双酚A的回收率最高(> 90%)。该方法在2~100μg·L^(-1)范围内呈良好线性关系,相关系数(r^2)大于0. 999,方法检出限(LOD)为0. 30~0. 52μg·L^(-1),定量下限(LOQ)为1. 00~1. 72μg·L^(-1),加标回收率为96. 5%~106%,相对标准偏差(RSD,n=7)为2. 0%~8. 6%。该法可满足欧盟指令(EU) 2017/898中双酚A迁移限量(0. 04 mg·L^(-1))的要求,且避免了因过滤器选择不当导致的双酚A损失,具有较好的实际意义。A reliable and sensitive method was developed for the determination of BPA migration in toys by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The migration conditions based on European toy safety standard EN 71-10:2005 with water as simulant were modified.The sample was filtrated with syringe filters made of mixed cellulose esters(MCE),then directly determined by HPLC-MS/MS.Furthermore,the influences of syringe filters were intensively investigated,and the MCE filters had satisfactory BPA recoveries larger than 90%,whereas other filters made of polyamide(PA,nylon 66)and polyether sulfone(PES)resulted in significant loss of BPA.There existed a good linearity of the method in the range of 2-100μg·L-1 with correlation coefficients(r 2)greater than 0.999.The limits of detection(LOD)were in the range of 0.30-0.52μg·L-1,and the limits of quantitation(LOQ)were 1.00-1.72μg·L-1.The spiked recoveries were in the range of 96.5%-106%with RSDs(n=7)of 2.0%-8.6%.The established method was successfully applied in the determination of migration of trace BPA in toys,avoiding the BPA loss caused by improper selection of syringe filters,which could meet the requirements for newly adopted BPA migration limit(0.04 mg·L-1)specified in the EU Directive 2017/898.

关 键 词：双酚A 迁移量 玩具 高效液相色谱-串联质谱法(HPLC-MS/MS) 

分 类 号：O657.63[理学—分析化学] O625.31[理学—化学]