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首页> 外文期刊>Journal of the Iranian Chemical Society >Ultrasound-assisted dispersive liquid-liquid microextraction method combined with HPLC-fluorescence detection for the determination of glycyrrhetinic acid in liquorice and liquorice-derived food products
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Ultrasound-assisted dispersive liquid-liquid microextraction method combined with HPLC-fluorescence detection for the determination of glycyrrhetinic acid in liquorice and liquorice-derived food products

机译:超声辅助液液微萃取-高效液相色谱-荧光检测法测定甘草及甘草食品中的甘草次酸

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摘要

A sensitive and inexpensive method involving ultrasound-assisted dispersive liquid-liquid microextraction (UA-DLLME) and pre-column derivatization followed by high-performance liquid chromatography with fluorescence detection (HPLC-FLD) was developed for the analysis of glycyrrhetinic acid. In this work, glycyrrhetinic acid could be obtained by hydrolyzing glycyrrhizic acid to remove glucuronic acid and subsequently extracted by UA-DLLME using chloroform and acetone as the extraction and disperser solvents, respectively. The sample extraction was firstly concentrated to dry under nitrogen and then rapidly derivatized with 2-(12-oxobenzo[b]acridin-5(12H)-yl)-ethyl-4-toluenesulfonate (BAETS) after the UA-DLLME. The prime parameters influencing the UA-DLLME and derivatization procedure were optimized using response surface methodology. Under the optimum conditions, the proposed method has a better linearity in a wider range of 6-300 ng mL(-1) and a high square of correlation coefficient (R (2)) at 0.9994. Limit of detection and limit of quantification were found to be 1.7 ng mL(-1) and 5.8 ng mL(-1), respectively. The proposed method was applied to the analysis of glycyrrhetinic acid in liquorice, liquorice apricot and sugar plum samples. For the analysis of the spiked samples, the spiked recoveries were in the range of 90.4-103.0 % with RSD less than 5.18 %. All results demonstrated that the UA-DLLME-HPLC-FLD (ultrasound-assisted dispersive liquid-liquid microextraction-high-performance liquid chromatography with fluorescence detection) was a sensitive, accurate, efficient analytical method for the determination of glycyrrhetinic acid.
机译:建立了一种灵敏且廉价的方法,该方法涉及超声辅助分散液-液微萃取(UA-DLLME)和柱前衍生化,然后进行高效液相色谱和荧光检测(HPLC-FLD),用于分析甘草次酸。在这项工作中,可以通过水解甘草次酸以去除葡萄糖醛酸来获得甘草次酸,然后分别使用氯仿和丙酮作为萃取和分散剂通过UA-DLLME进行萃取。样品萃取首先在氮气下浓缩至干,然后在UA-DLLME之后用2-(12-氧代苯并[b] ac啶-5(12H)-基)-4-甲苯磺酸乙酯(BAETS)快速衍生化。使用响应面方法对影响UA-DLLME和衍生化过程的主要参数进行了优化。在最佳条件下,该方法在6-300 ng mL(-1)的较宽范围内具有较好的线性,并且在0.9994处具有较高的相关系数平方(R(2))。检出限和定量限分别为1.7 ng mL(-1)和5.8 ng mL(-1)。该方法用于甘草,甘草杏和李子样品中的甘草次酸的分析。对于加标样品的分析,加标回收率在90.4-103.0%的范围内,RSD小于5.18%。所有结果表明,UA-DLLME-HPLC-FLD(超声辅助分散液-液微萃取-高效液相色谱-荧光检测)是一种灵敏,准确,高效的测定甘草次酸的分析方法。

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