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首页> 外文期刊>Food Chemistry >Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography
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Optimisation of ultrasound-assisted reverse micelles dispersive liquid-liquid micro-extraction by Box-Behnken design for determination of acetoin in butter followed by high performance liquid chromatography

机译:应用Box-Behnken设计优化超声辅助反胶束分散液-液微萃取法测定黄油中的乙醛,然后进行高效液相色谱法

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摘要

A novel approach, ultrasound-assisted reverse micelles dispersive liquid-liquid microextraction (USA-RM-DLLME) followed by high performance liquid chromatography (HPLC) was developed for selective determination of acetoin in butter. The melted butter sample was diluted and homogenised by n-hexane and Triton X-100, respectively. Subsequently, 400 μL of distilled water was added and the microextraction was accelerated by 4 min sonication. After 8.5 min of centrifugation, sedimented phase (surfactant-rich phase) was withdrawn by microsyringe and injected into the HPLC system for analysis. The influence of effective variables was optimised using Box-Behnken design (BBD) combined with desirability function (DF). Under optimised experimental conditions, the calibration graph was linear over the range of 0.6-200 mg L~(-1). The detection limit of method was 0.2 mg L~(-1) and coefficient of determination was 0.9992. The relative standard deviations (RSDs) were less than 5% (n = 5) while the recoveries were in the range of 93.9-107.8%.
机译:开发了一种超声辅助反胶束分散液-液微萃取(USA-RM-DLLME),然后进行高效液相色谱(HPLC)的新方法,用于选择性测定黄油中的乙酰丙酮。将熔融的黄油样品分别用正己烷和Triton X-100稀释并均质化。随后,添加400μL蒸馏水,并通过超声处理4分钟加速微萃取。离心8.5分钟后,通过微注射器抽出沉淀相(富含表面活性剂的相),并注入HPLC系统进行分析。有效变量的影响使用Box-Behnken设计(BBD)结合期望函数(DF)进行了优化。在优化的实验条件下,校准曲线在0.6-200 mg L〜(-1)范围内呈线性关系。该方法的检出限为0.2 mg L〜(-1),测定系数为0.9992。相对标准偏差(RSD)小于5%(n = 5),而回收率在93.9-107.8%的范围内。

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