Simultaneous determination of trace migration of phthalate esters in honey and royal jelly by GC-MS.
Simultaneous determination of trace migration of phthalate esters in honey and royal jelly by GC-MS.
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DOI：
10.1002/jssc.201300778
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发表时间：
2014-03
影响因子：
3.1
通讯作者：
Jinhui Zhou;Yitao Qi;Hongmei Wu;Q. Diao;Feifei Tian;Yi Li
中科院分区：
文献类型：
--
作者：
Jinhui Zhou;Yitao Qi;Hongmei Wu;Q. Diao;Feifei Tian;Yi Li
建立了一种简便、快速、可靠的液-液萃取-气相色谱-质谱联用方法，用于蜂蜜和皇家浆中22种邻苯二甲酸酯（PAEs）的定量分析。对GC-MS的仪器参数进行了测试，获得了22种邻苯二甲酸酯的满意分离，具有较高的灵敏度。为了达到最佳回收率，对提取程序进行了优化。采用以下标准验证开发的方法：线性、LOD、LOQ下限、精密度、准确度、基质效应和残留。通过应用基于最小二乘法的线性回归模型和加权因子（1/x），相关系数>0.999。日内和日间精密度的RSD均在12.7%以内，准确度的相对误差均在-11.8%以内。蜂蜜和皇家浆的平均提取回收率在80.1和110.9%之间。蜂蜜和皇家浆样品的分析没有观察到显着的基质效应和携带的邻苯二甲酸酯。共20个真实的样本进行了分析，使用开发的方法进行小型调查。在蜂蜜样品中发现了7种邻苯二甲酸酯，在皇家浆样品中发现了5种邻苯二甲酸酯，表明可能受到几种邻苯二甲酸酯的污染。
A simple, rapid, and reliable liquid-liquid extraction coupled to GC-MS method was developed and validated for the quantification of 22 phthalate esters (PAEs) in honey and royal jelly. Instrument parameters for GC-MS were tested to obtain the satisfactory separation between 22 PAEs with high sensitivity. The extraction procedure was optimized in order to achieve the best recovery. The following criteria were used to validate the developed method: linearity, LOD, lower LOQ, precision, accuracy, matrix effect and carry-over. Correlation coefficients were >0.999 by applying the linear regression model based on the least-squares method with a weighting factor (1/x). The intra- and interday precision were within 12.7% in terms of RSD, and the accuracy was within -11.8% in terms of relative error. The mean extraction recoveries ranged between 80.1 and 110.9% for honey and royal jelly. No significant matrix effect and carry-over for PAEs were observed for the analysis of honey and royal jelly samples. A total of 20 real samples were analyzed for a mini-survey using the developed method. Seven PAEs in honey samples and five PAEs in royal jelly samples were found, indicating potential contamination with several PAEs.