State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, PR China.
J Sep Sci. 2010 Feb;33(2):251-7. doi: 10.1002/jssc.200900557.
In this study, a simple, rapid and sensitive method for the determination of five phthalates including dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzyl butyl phthalate, and dicyclohexyl phthalate in fruit jellies by LC coupled with MS has been developed. Samples were pretreated by a dispersive SPE method, termed QuEChERS, which is an acronym for quick, easy, cheap, effective, rugged, and safe. The standard calibration curves were linear for all the analytes over the concentration range of 10-250 ng/mL, and the correlation coefficients ranged from 0.9976 to 0.9991. The LODs and LOQs were in the ranges of 0.09-3.68 ng/mL and 0.28-11.25 ng/mL, respectively. The accuracy of this method was evaluated by measuring the recovery from spiked samples. The recoveries of all five phthalates from samples spiked at three different concentrations (0.01, 0.03, and 0.05 mg/kg), were in the ranges of 83.5-103.9%, 86.7-95.8%, and 87.1-95.2%, respectively. The RSD values for the samples spiked at 0.01, 0.03, and 0.05 mg/kg ranged from 2.0-7.6%, 1.4-6.4%, and 1.2-3.8%, respectively. The method has been used for the analysis of real samples and BBP and DEP were found in real samples.
本研究建立了一种简单、快速、灵敏的 LC-MS 法，用于测定果冻中的五种邻苯二甲酸酯，包括邻苯二甲酸二甲酯、邻苯二甲酸二乙酯、邻苯二甲酸二丙酯、邻苯二甲酸丁基苄基酯和邻苯二甲酸二环己酯。样品采用 QuEChERS 法（即快速、简单、廉价、有效、耐用、安全）进行分散固相萃取预处理。所有分析物在 10-250 ng/mL 浓度范围内的标准校准曲线均呈线性，相关系数范围为 0.9976-0.9991。检出限和定量限分别为 0.09-3.68 ng/mL 和 0.28-11.25 ng/mL。该方法的准确性通过测量加标样品的回收率进行评估。五种邻苯二甲酸酯在三个不同浓度（0.01、0.03 和 0.05 mg/kg）的加标样品中的回收率分别为 83.5-103.9%、86.7-95.8%和 87.1-95.2%。在 0.01、0.03 和 0.05 mg/kg 加标水平下，样品的 RSD 值范围分别为 2.0-7.6%、1.4-6.4%和 1.2-3.8%。该方法已用于实际样品的分析，并在实际样品中发现了 BBP 和 DEP。
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