摘要
建立了采用高效液相色谱·质潜联用法(Lc-MS.Ms)测定玩具材料中总量双酚A的检测方法。样品经二氯甲烷萃取,通过旋转蒸发仪进行净化后,采用C18柱,以甲醇-水混合液为流动相,等比例洗脱分离,经串联四级杆质谱仪在负离子模式下以多反应监测模式进行检测。结果表明:该方法在0.01-10mg/L范围内线性关系良好,线性方程的相关系数r2=0.9993。该方法的检出限为0.005mg/kg;在20ml啦g、50mg/kg和80mg/kg三个添加浓度水平下t玩具材料中双酚A的平均回收率为76.8%~99.0%。相对标准偏差(n=:6)均小于10.0%。该方法操作简便,灵敏度高,适用于玩具原材料、玩具及儿童产品部件中双酚A的总含量测定。
A comprehensive analytical method based on high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed for bisphenol A from toys material. The sample was extracted with dichloromethane. Sample concentration and purification was performed on rotary evaporator. And then, the separation compound was analyzed with a ZORBAX Eclipse Plus C18 column by isocratic elution with methyl alcohol- H20 as mobile phase. After gradient elution separation, the analyte was detected under multiple reaction monitoring (MRM) with electrospry ionization in negative ion mode (ESI-). The calibration curves for bisphenol A was linear in the range of 0.01-10 mg/L and the correlation coefficient were 0.9993. The quantitation limit was 0.005 mg/kg. The mean recoveries at three spiked concentration levels of 20 mg/kg, 50 mg/kg, 80 mg/kg were in the range of 76.8 %-99.0 % with RSDs(n=6) less than 10 %. This method is simple, accurate and rapid, and is suitable for the inspection of bisphenol A from toy materials.
出处
《广东化工》
CAS
2013年第12期172-173,共2页
Guangdong Chemical Industry