Inspection and Quarantine Technology Center, Xiamen Entry-Exit Inspection and Quarantine Bureau, Xiamen 361026, China.
Animal Plants & Foods Inspection and Quarantine Technical Center, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China.
J Chromatogr A. 2014 Jan 10;1324:49-56. doi: 10.1016/j.chroma.2013.11.017. Epub 2013 Nov 20.
A rapid and sensitive method was developed for the determination of 23 phthalates in food samples including milk-based products, distilled liquor, wine, beverage, grain, meat, oil, biscuit (cookie), and canned food by liquid chromatography tandem mass spectrometry (LC-MS/MS). Liquid samples were exacted by acetonitrile, while solid samples were prepared by QuEChERS or glass-based SPE methods. The 23 phthalates were separated on Poroshell 120 EC-C18 column and followed by positive electrospray ionization as well as multi-reaction monitoring provided by a triple-quadrupole tandem mass spectrometer. To reduce contamination, the plastic materials were avoided in sample handling and preparation . The LODs were between 0.8 and 15 μg kg(-1) and LOQs were between 10 and 100 μg kg(-1). By using different concentrations: 100, 500, and 1000 μg kg(-1)) for DINP and DIDP; 50, 100, and 1000 μg kg(-1) for other 21 phthalate compounds, the spiked recoveries were within 75.5-115.2% and the relative standard deviations (RSDs) were in the range of 3.2-18.9%. The proposed protocol was then applied to the analysis of 623 real samples collected from the two sides of the Taiwan Straits, and the DEHP was found in almost all samples tested in this study, with levels ranging from 0.02 to 2685 mg kg(-1). The present study demonstrated a rapid, sensitive, and accurate method for determining 23 phthalates in foodstuffs.
建立了一种快速、灵敏的液相色谱串联质谱法测定乳基产品、蒸馏酒、葡萄酒、饮料、谷物、肉类、油脂、饼干（曲奇）和罐头食品中 23 种邻苯二甲酸酯的方法。液体样品用乙腈提取，固体样品用 QuEChERS 或基于玻璃的 SPE 方法制备。23 种邻苯二甲酸酯在 Poroshell 120 EC-C18 柱上分离，采用正电喷雾电离和三重四极杆串联质谱仪提供的多反应监测模式。为了减少污染，在样品处理和制备过程中避免使用塑料材料。方法的检出限（LOD）在 0.8-15μg/kg 之间，定量限（LOQ）在 10-100μg/kg 之间。使用不同浓度（DINP 和 DIDP 为 100、500 和 1000μg/kg；其他 21 种邻苯二甲酸酯化合物为 50、100 和 1000μg/kg）对样品进行加标回收实验，加标回收率在 75.5%-115.2%之间，相对标准偏差（RSD）在 3.2%-18.9%之间。该方法应用于海峡两岸 623 个实际样品的分析，结果表明，在所检测的样品中几乎都检出了 DEHP，含量范围为 0.02-2685mg/kg。本研究建立了一种快速、灵敏、准确的测定食品中 23 种邻苯二甲酸酯的方法。
