三种糖品中植物甾醇的测定  

Determination of phytosterols in three kinds of sugar

作　　者：陈其钊 林燕纯 刘志鹏 陈嘉敏 李长成 王桂华 李家威 余构彬 CHEN Qizhao;LIN Yanchun;LIU Zhipeng;CHEN Jiamin;LI Changcheng;WANG Guihua;LI Jiawei;YU Goubin(Guangdong Provincial Bioengineering Institute(Guangzhou Suga rcane Industry Research Institute)China Sugar Inspection Center,Guangzhou 510316,China;Shantou Prokayong Biomedical Technology Co.,Ltd.,Shantou 515000,China)

机构地区：[1]广东省生物工程研究所(广州甘蔗糖业研究所)国家糖业质量监督检验中心,广东广州510316 [2]汕头普罗凯融生物医药科技有限公司,广东汕头515000

出　　处：《食品与发酵工业》2020年第22期238-244,共7页Food and Fermentation Industries

基　　金：广州市科技计划项目(201806010093)。

摘　　要：建立了采用高效液相色谱-二极管阵列检测器法测定红糖、黑糖和赤砂糖中5种植物甾醇的方法。样品经无水乙醇涡旋提取后水浴皂化,用二氯甲烷萃取氮气吹干后甲醇复溶。用Waters ACQUITY UPLC BEH C8液相色谱柱(2.1 mm×100 mm,1.7μm),以乙腈和水溶液为流动相,流速为0.4 mL/min,柱温为35℃,进样量为5μL,二级管阵列检测器检测范围为190~810 nm,检测波长为205、282 nm。麦角甾醇,胆甾醇,菜油甾醇,豆甾醇,β-谷甾醇在0.1~100μg/mL浓度范围内线性相关系数r^2为0.9997~0.9999,方法检出限分别为0.023,0.14,0.18,0.11和0.17 mg/kg。3个浓度加标水平的回收率为74.4%~102.5%,相对标准偏差为0.1%~3.6%。样品测定结果表明,3种糖品中5种甾醇含量与总甾醇含量差异明显,总体分布为红糖>黑糖>赤砂糖。该方法前处理简单,灵敏度高,重现性和回收率好,具有良好的精密度和准确度,可用于糖品中5种植物甾醇分析检测。A method for the determination of five phytosterols in brown sugar,dark brown sugar and brown granulated sugar by high performance liquid chromatography with diode array detector was established.The sample was extracted by anhydrous ethanol,then saponified in water bath;after that the sample was extracted with dichloromethane,dried with nitrogen and then dissolved with methanol.A Waters ACQUITY UPLC BEH C 8 liquid chromatographic was used for the detection with the following conditions:Column(2.1 mm×100 mm,1.7μm);acetonitrile and aqueous solution were used as mobile phase with the flow rate 0.4 mL/min and the column temperature at 35℃;the injection volume was 5μL and the detection range of diode array detector was 190-810 nm;the detection wavelength was 205 and 282 nm.The results showed that the linear correlation coefficients of ergosterol,cholesterol,rapeseed oil sterol,stigmasterol andβ-sitosterol in the concentration range of 0.1-100μg/mL were 0.9997 and 0.9999,respectively.The detection limits of the method were 0.023,0.14,0.18,0.11 and 0.17 mg/kg.The recovery rate of the three concentration addition levels was 74.4%-102.5%,and the relative standard deviation is 0.1%-3.6%.The results of sample determination showed that the contents of five sterols and total sterols in the three sugars were significantly different.The overall distribution was brown sugar>dark brown sugar>brown granulated sugar.The method developed here has the advantages of simple pretreatment,high sensitivity,good reproducibility and recovery,good precision and accuracy,and can be used for the analysis and detection of five kinds of phytosterols in sugar.

关 键 词：红糖 黑糖 赤砂糖 植物甾醇 液相色谱法 

分 类 号：O657.72[理学—分析化学] TS247[理学—化学]