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分散液液微萃取在实际样品中八种对羟基苯甲酸酯的预浓缩及其高效液相色谱法测定。

Application of dispersive liquid-liquid microextraction for the preconcentration of eight parabens in real samples and their determination by high-performance liquid chromatography.

机构信息

Department of Pharmacy, Zhongshan Hospital, Fudan University, Shanghai, P.R. China.

Shanghai Institute for Food and Drug Control, Shanghai, P.R. China.

出版信息

J Sep Sci. 2017 Nov;40(22):4385-4393. doi: 10.1002/jssc.201700722. Epub 2017 Sep 26.

Abstract

A simple and sensitive method for the simultaneous determination of eight parabens in human plasma and urine samples was developed. The samples were preconcentrated using dispersive liquid-liquid microextraction based on the solidification of floating organic drops and determined by high-performance liquid chromatography with ultraviolet detection. The influence of variables affecting the extraction efficiency was investigated and optimized using Placket-Burman design and Box-Behnken design. The optimized values were: 58 μL of 1-decanol (as extraction solvent), 0.65 mL methanol (as disperser solvent), 1.5% w/v NaCl in 5.0 mL of sample solution, pH 10.6, and 4.0 min centrifugation at 4000 rpm. The extract was injected into the high-performance liquid chromatography system for analysis. Under the optimum conditions, the linear ranges for eight parabens in plasma and urine were 1.0-1000 ng/mL, with correlation coefficients above 0.994. The limit of detection was 0.2-0.4 and 0.1-0.4 ng/mL for plasma and urine samples, respectively. Relative recoveries were between 80.3 and 110.7%, while relative standard deviations were less than 5.4%. Finally, the method was applied to analyze the parabens in 98 patients of primary breast cancer. Results showed that parabens existed widely, at least one paraben detected in 96.9% (95/98) of plasma samples and 98.0% (96/98) of urine samples.

摘要

建立了一种用于同时测定人血浆和尿液样品中 8 种对羟基苯甲酸酯的简单灵敏的方法。该方法基于固-液萃取技术,采用分散液-液微萃取对样品进行预处理,然后采用高效液相色谱-紫外检测法进行测定。通过 Placket-Burman 设计和 Box-Behnken 设计考察并优化了影响萃取效率的变量。优化后的条件为:萃取溶剂 1-癸醇 58 μL,分散溶剂甲醇 0.65 mL,样品溶液中 5.0 mL 含 1.5%(w/v)NaCl,pH 值 10.6,4000 r/min 离心 4.0 min。将萃取物注入高效液相色谱系统进行分析。在最佳条件下,8 种对羟基苯甲酸酯在血浆和尿液中的线性范围分别为 1.0-1000 ng/mL,相关系数均大于 0.994。对血浆和尿液样品的检测限分别为 0.2-0.4 和 0.1-0.4 ng/mL。相对回收率在 80.3%至 110.7%之间,相对标准偏差均小于 5.4%。最后,该方法应用于 98 例原发性乳腺癌患者的对羟基苯甲酸酯分析。结果表明,对羟基苯甲酸酯广泛存在,96.9%(95/98)的血浆样品和 98.0%(96/98)的尿液样品中至少检测到 1 种对羟基苯甲酸酯。

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