花椒游离脂肪酸的微波快速提取与衍生化HPLC荧光检测方法研究  

Microwave rapid extraction of free fatty acids from Zanthoxylum bungeanum Maxim and their HPLC fluorescence detection by pre-column derivatization

作　　者：郑振佳[1] 席兴军[1] 赵先恩[2] 赵镭[1] 张璐璐[1] 郑佳佳[1] 

机构地区：[1]中国标准化研究院食品与农业标准化研究所,北京100088 [2]曲阜师范大学化学与化工学院,山东曲阜273165

出　　处：《食品工业科技》2013年第14期58-62,共5页Science and Technology of Food Industry

基　　金：国家自然科学基金项目(31171695);质检公益性行业科研专项(201210216)

摘　　要：建立了花椒中游离脂肪酸的微波快速提取技术,并采用苯并[b]吖啶酮-5-乙基对甲苯磺酸酯(BAETS)作为柱前衍生试剂,建立了19种长链饱和与不饱和游离脂肪酸的衍生化HPLC荧光检测分析方法。微波提取功率700W,溶剂为体积比1∶1的氯仿/甲醇,70℃提取10min,可达近100%提取率。采用色谱柱Eclipse XDB-C8(4.6mm×150mm,5μm),酸性乙腈/水流动相进行梯度洗脱,HPLC荧光激发和发射波长分别为273nm和505nm。同时进行在线质谱辅助鉴定(APCI-MS),更提高了HPLC荧光定量的准确度。结果表明,微波提取快速高效,分析方法线性良好,线性范围14.286～0.0139μmol/L,最低检出限为0.636nmol/L,回收率在87.60%～106.59%之间。本方法快速、准确、高灵敏,可作为花椒相关样品的标准化检测方法。Free fatty acids（FFAs） in Zanthoxylum bungeanum Maxim were extracted by microwave-assisted extraction and derivatized using 2- （ 12-oxobenzo[b]acridin-5 （ 12H ） -yl ） ethyl-4-toluenesulfonate （BAETS） as derivatization reagent. This method was proposed to detect 19 long-chain saturated and unsaturated FFA derivatives by HPLC fluorescence detection using pre-column derivatization. Microwave-assisted extract percentages almost reached 100% when FFAs were extracted at microwave power 700W,70~C and 10min using chloroform/methanol（1：1 ,v：v）. Good chromatographic separation was achieved using acidic acetonitrile/ water as mobile phase on Eclipse XDB-C8 column（4.6mm×150mm,5μm） by gradient elution. On-line APCI- MS identification was used for producing more accurate HPLC fluorescence quantitation. Fluorescence excitation and emission wavelengths for HPLC detection were 273nm and 505nm,respectively. The results indicated that microwave-assisted extraction was fast and efficient,and the developed analytical method had good linearity. Linear range was from 14.286 to 0.0139μmol/L,the lowest detection limits was 0.636nmol/L,the recovery was in the range of 87.60%-106.59%. The established method was rapid,accurate,and highly sensitive, it can be used as standardized detection method for free fatty acids.

关 键 词：花椒 游离脂肪酸 微波提取 衍生化 HPLC荧光检测 

分 类 号：TS207.3[轻工技术与工程—食品科学]