高效液相色谱-串联质谱法检测玩具中5种香豆素类致敏性香味剂  

Determination of five coumarins in toys by high performance liquid chromatography-tandem mass spectrometry

作　　者：杨荣静[1] 卫碧文[1] 高欢[1] 于文佳[1] 

机构地区：[1]上海出入境检验检疫局,上海200135

出　　处：《色谱》2012年第2期160-164,共5页Chinese Journal of Chromatography

摘　　要：建立了一种简单、快速、准确测定玩具中香豆素、7-甲氧基香豆素、二氢香豆素、7-甲基香豆素、7-乙氧基-4-甲基香豆素5种香豆素类致敏性香味剂的检测方法。样品经四氢呋喃超声提取,提取液浓缩至近干,以25 mL甲醇溶解残渣定容后进行高效液相色谱-串联质谱分析。色谱流动相为乙腈和0.1%乙酸水溶液,梯度洗脱,多反应监测(MRM)模式进行定性和定量分析。5种目标物的工作曲线线性范围均为10～1 000μg/L;除了二氢香豆素的定量限(信噪比(S/N)>10)为5.0μg/L外,其他化合物均为2.0μg/L;在3种不同类型的样品中添加高、中、低水平的5种目标物标准品,其加标回收率为93.2%～105.8%,相对标准偏差为3.65%～8.27%。应用本方法对12种玩具和儿童用品样品进行了测试,其中9个样品中检出了香豆素类致敏性香味剂,有两个样品中香豆素和7-甲氧基香豆素的含量超过了欧盟玩具新指令的限量要求。A rapid analytical method for the determination of five coumarins（coumarin,7-methoxycoumarin,dihydrocoumarin,7-methyl coumarin and 7-ethoxy-4-methyl coumarin） in toys by high performance liquid chromatography-tandem mass spectrometry（HPLC-MS/MS） has been developed.After ultrasonic extraction in tetrahydrofuran,the samples were analyzed by HPLC-MS/MS in multi-reaction monitoring（MRM） mode.Acetonitrile and 0.1% acetic acid were used as the mobile phases with gradient elution.The linear ranges of calibration curves were 10-1 000 μg/L,and the limits of quantification（LOQ）（S/N10） were 2.0 μg/L for all the analytes,except that the LOQ for dihydrocoumarin was 5.0 μg/L.The recoveries of the five coumarins spiked in three types of samples were in the ranges of 93.2%-105.8%,97.3%-103.2% and 96.8%-102.9%,with the relative standard deviations in the ranges of 4.35%-8.27%,3.65%-6.73% and 4.03%-6.45%,respectively.The method was applied in the determination of 12 toy samples.The five analytes were found in 9 samples,and in some cases,the presence of quite high concentrations of these coumarins in the toys should be a matter of concern.

关 键 词：高效液相色谱-串联质谱 香豆素 致敏性香味剂 玩具 

分 类 号：O658[理学—分析化学]