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首页> 外文期刊>The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry >Development of molecularly imprinted poly(methacrylic acid)/silica for clean-up and selective extraction of cholesterol in milk prior to analysis by HPLC-UV
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Development of molecularly imprinted poly(methacrylic acid)/silica for clean-up and selective extraction of cholesterol in milk prior to analysis by HPLC-UV

机译：分子印迹聚（甲基丙烯酸）/二氧化硅的开发，用于在HPLC-UV分析之前净化和选择性提取牛奶中的胆固醇

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摘要

In the present paper the assessment of a novel molecularly imprinted polymer, poly(methacrylic acid)/silica, for clean-up and selective extraction of cholesterol in milk samples is described. The relative selectivity coefficient (k) values for cholesterol/5-a-cholestane and cholesterol/7-dehydrocholesterol systems were found to be 5.08 and 6.08, respectively, thus attesting the selectivity of the MIP for cholesterol under competitive adsorption with structurally analogous steroid compounds. The milk analysis was initially based on saponification followed by liquid–liquid extraction with n-hexane. Then, the protocol of molecularly imprinted solid phase extraction (MISPE) was carried out by loading the milk hexanic extract through 200 mg of MIP or NIP (non-imprinted polymer) packed into SPE cartridges at a flow rate of 0.6 mL min~(-1). The washing step was performed by using n-hexane followed by further elution with ethanol and HPLC-UV analysis at 208 nm. From the breakthrough curve the maximum adsorption capacity of the MIP towards cholesterol was found to be 29.51 mg g~(-1). The precision of the MISPE protocol was assessed as intra- and inter-days yielding RSD (relative standard deviations) lower than 4.10%. Cleaner HPLC chromatograms were obtained for milk samples submitted to the MISPE protocol in comparison to the solid phase extraction using the NIP or modified octadecyl silica (C_(18)). Recoveries varying from 96.6 up to 102.2% for milk samples spiked with cholesterol were achieved, thus ensuring the accuracy of the proposed method.
机译：在本文中，描述了一种用于清洁和选择性提取牛奶样品中胆固醇的新型分子印迹聚合物聚（甲基丙烯酸）/二氧化硅的评估。发现胆固醇/5-α-胆甾烷和胆固醇/ 7-脱氢胆固醇体系的相对选择性系数（k）值分别为5.08和6.08，从而证明了在与结构类似的类固醇化合物竞争性吸附下，MIP对胆固醇的选择性。 。牛奶分析最初是基于皂化作用，然后用正己烷进行液-液萃取。然后，通过将牛奶己酸提取物通过0.6 mg min〜（-）的200 mg MIP或NIP（非印迹聚合物）装入SPE柱中，进行分子印迹固相萃取（MISPE）的操作。 1）。通过使用正己烷进行洗涤步骤，然后进一步用乙醇洗脱和在208nm下进行HPLC-UV分析。从穿透曲线可知，MIP对胆固醇的最大吸附量为29.51 mg g〜（-1）。 MISPE协议的精度评估为日内和日间得出的RSD（相对标准偏差）低于4.10％。与使用NIP或改性十八烷基二氧化硅（C_（18））进行固相萃取相比，提交MISPE规程的牛奶样品获得了更清洁的HPLC色谱图。对于加有胆固醇的牛奶样品，回收率从96.6到102.2％不等，从而确保了所提出方法的准确性。

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