高效液相色谱—串联质谱法检测玩具中的壬基酚和辛基酚  

Simultaneous Determination of Nonylphenol and Octylphenol from Rubber Toys by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：李小莹[1] 李琼[1] 刘华鼐[1] 

机构地区：[1]华南理工大学化学与化工学院,广东广州510641

出　　处：《广东化工》2016年第14期212-213,215,共3页Guangdong Chemical Industry

摘　　要：建立了儿童玩具中的壬基酚和辛基酚的高效液相色谱串联质谱分析方法。样品用甲醇微波提取,采用ZORBAX Eclipse Plus C18色谱柱,以甲醇-水为流动相,等梯度洗脱分离后,串联四极杆质谱多反应监测方式检测,以保留时间和相对离子丰度（离子比率）定性,外标法定量。在优化条件下,该方法 5 min内即可完成待测物的分析。壬基酚和辛基酚在0.001-0.10 mg/L的范围内线性关系良好,相关系数大于0.999,方法的定量下限为0.02 mg/kg。在加标水平为0.02、0.2、2.0 mg/kg时,待测物的平均加标回收率为76.8%-99.0%,相对标准偏差（n=6）小于6.6%。该方法准确、快速、灵敏,适用于儿童玩具中的壬基酚和辛基酚的快速确认和定量检测。A comprehensive analytical method based on high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） has been developed for nonylphenol and octylphenol from toys. The homogenized samples were extracted with methanol using microwave method and separated with a ZORBAX Eclipse Plus C18 column with MeOH-H20 as mobile phase. After equivalent elution separation, the analytes were detected under multiple reaction monitoring （MRM） with electrospry ionization in negative ion mode （ESI-）. The analytes were identified by retention times and ion ratios, and quantified by the external standard method. Under the optimal conditions, the separation of analytes was performed within 5 min. The calibration curves for 2 compounds were linear in the range of 0.001-0.10 mg/k with correlation coefficients more than 0.999. The quantitation limits of this method was 0.02 mg/kg. The mean recoveries for two compounds at three spiked concentration levels of 0.02, 0.2, 2.0 mg/kg were in the range of 76.8 %-99.0 % with RSDs （n=6） less than 6.6 %. The average spiked recoveries ranged from 76 % to 96 % （RSD〈6.6 %）. Themethod is accurate, simple and rapid, and is suitable for the inspection of the nonylphenol and octylphenol.

关 键 词：玩具 液相色谱串联质谱法 壬基酚 辛基酚 

分 类 号：O65[理学—分析化学]