The application of directly suspended droplet microextraction for the evaluation of phthalic acid esters in cow's milk by gas chromatography mass spectrometry.
The application of directly suspended droplet microextraction for the evaluation of phthalic acid esters in cow's milk by gas chromatography mass spectrometry.
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DOI：
10.1016/j.chroma.2016.03.062
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发表时间：
2016-04
期刊：
影响因子：
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通讯作者：
Dan Liu;S. Min;Hua Ping;Xiang-zhong Song
中科院分区：
文献类型：
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作者：
Dan Liu;S. Min;Hua Ping;Xiang-zhong Song
采用直接悬浮液滴微萃取-气相色谱-质谱联用技术（DSDME-GC-MS），建立了一种简便、快速测定牛奶中16种邻苯二甲酸酯（PAEs）的方法。优化了萃取和DSDME实验的不同参数，包括：三氯乙酸浓度10 g/L，环己烷微滴有机溶剂100 μL，搅拌速度1100 rpm，萃取时间10 min，无盐量。方法的线性范围为γ > 0.9878，0.002-0.4 μg/mL，精密度（RSD < 11%）和准确度（相对回收率为70.2 ~ 108%）均较好。15种邻苯二甲酸酯的检测限（LOD）范围为0.001 - 0.2 μg/L，定量限（LOQ）范围为0.003 - 0.7 μg/L。邻苯二甲酸二壬酯（DINP）的响应较低，线性不好。该方法已成功应用于真实的牛奶样品中邻苯二甲酸酯的分析。
A simple and rapid method was developed for evaluating 16 phthalic acid esters (PAEs) at the μg/kg level in a complex milk matrix using directly suspended droplet microextraction-gas chromatography mass spectrometry (DSDME-GC–MS). The different parameters for extraction and for the DSDME experiment were optimized, including You are free to submit the revised manuscript at a later date as a new submission.10 g/L trichloroacetic acid concentration, 100 μL cyclohexane micro-droplet organic solvent, 1100 rpm stirring speed, 10 min extraction time and no salt amount. Validation experiments showed good linearity (γ > 0.9878, 0.002–0.4 μg/mL), satisfactory precision (RSD < 11%), and good accuracy (relative recovery of 70.2–108%) when analyzing milk samples using the optimized method. The limits of detection (LODs) ranged between 0.001 and 0.2 μg/L, and the limits of quantification (LOQs) ranged between 0.003 and 0.7 μg/L for 15 PAEs. Dinonyl phthalate (DINP) had a low response and did not have good linearity. The proposed method was successfully applied for the analysis of PAEs in real milk samples.