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超声辅助分散液液微萃取-气相色谱法同时测定瓶装奶中 6 种邻苯二甲酸酯

Simultaneous determination of six phthalate esters in bottled milks using ultrasound-assisted dispersive liquid-liquid microextraction coupled with gas chromatography.

机构信息

Key Laboratory of Pharmaceutical Quality Control of Hebei Province & College of Pharmacy, Hebei University, Baoding 071002, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Sep 1;879(25):2507-12. doi: 10.1016/j.jchromb.2011.07.001. Epub 2011 Jul 12.

Abstract

A new method was developed for the simultaneous determination of six phthalate esters in bottled milks using ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) followed by gas chromatography-flame ionization detection (GC-FID). 0.8 mL of methanol (dispersant) and 40 μL of CCl(4) (extractant) were injected into 8.0 mL of milk solution and then emulsified the mixture by ultrasound for 2.0 min to form the cloudy solution. Under the optimum condition, the enrichment factors of the analytes ranged from 220 to 270 fold and the recovery ranged from 93.2% to 105.7%. Good linearity was observed for all analytes in a range of 0.8-51 ngg(-1) with the correlation coefficient (r(2)) ≥ 0.9992. The limits of detection (LODs) based on signal to noise of 3 were 0.64-0.79 ngg(-1). The repeatability evaluated as intra-day and inter-day precision (relative standard deviation, RSD) were less than 4.0% (n=5). The presented UA-DLLME-GC-FID method was successfully applied to determine the six phthalate esters in different bottled milk products.

摘要

建立了超声辅助分散液-液微萃取(UA-DLLME)-气相色谱-火焰离子化检测(GC-FID)联用测定瓶装奶中 6 种邻苯二甲酸酯的新方法。将 0.8 mL 甲醇(分散剂)和 40 μL CCl4(萃取剂)注入 8.0 mL 奶样中,超声乳化 2.0 min 形成混浊溶液。在最佳条件下,目标物的富集因子为 220270 倍,回收率为 93.2%105.7%。所有目标物在 0.851 ng/g 范围内均具有良好的线性关系,相关系数(r2)≥0.9992。基于信噪比为 3 的检出限(LOD)为 0.640.79 ng/g。日内和日间精密度(相对标准偏差,RSD)小于 4.0%(n=5)。所建立的 UA-DLLME-GC-FID 方法成功用于不同瓶装奶中 6 种邻苯二甲酸酯的测定。

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