摘要
建立了一种新的测定酿酒葡萄中赭曲霉毒素A含量的方法——“葡萄皮-SPE-HPLC”法：将酿酒葡萄剥皮后用0．1mol／L磷酸-二氯甲烷（1：10）提取；取10mL提取液进样固相萃取小柱，0．1mol／L磷酸、双蒸水淋洗，乙酸乙酯洗脱后吹干，流动相溶解；高效液相色谱法测定条件为C18反相柱分离，乙腈-水-乙酸（体积比99：99：2）为流动相，荧光检测器（激发波长330nm，发射波长460nm）检测。该方法回收率为102％～109％，变异系数为0．1％～2．0％；用此方法检测贺兰山东麓“玉泉营”和“万义山庄”两个产地酿酒葡萄中OTA含量，结果介于5～10μg／kg，均有一定程度赭曲霉毒素A污染。
The new method for determination of Ochratoxin A in grape established in this paper named ＂Pericarp- SPE-HPLC＂. The fresh wine grape was peeled. Ochratoxin A was extracted from grape pericarp with 0. 1M phosphoric acid- dichloromethane （1： 10）. After C18 solid phase extraction column （C18-SPE） has activated with 5mL Methanol, 5mL double diluted water, and 5mL Sodium hydrogen carbonate （30g/L） , the above extract 10mL was firstly brought into C18-SPE column. Then the C18-SPE column was washed with 2mL phosphoric acid （0.1mol/L） and 2mL double distilled water respectively and was eluted with 5mL ethyl acetate subsequently. The eluent was dried with Nz gas. The residue was dissolved with 0.2 mL of mobile phase for determination. The chromatographic column was C18 reversed-phase column（ 150 mm ×4.6 mm i. d. ）for separation. Mobile phase was acetonitrile-water-acetic acid （99： 99： 2）. A high performance liquid chromatography was determined with fluorescence detection. The excitation wavelength was 330nm. The emission wavelength was 460 nm. The recoveries of this method were between 102.5% and 109.7% , and coefficient of variation varied from 0. 14% to 2.07%. Results from analysis with ＂Pericarp-SPE- HPLC＂ method showed that Ochratoxin A in two grape samples ＂yuquanying＂ and ＂wanyi heights＂ were 5 - 10 μg/ kg.
出处
《食品与发酵工业》
CAS
CSCD
北大核心
2013年第9期175-179,共5页
Food and Fermentation Industries
基金
宁夏自然科学基金:贺兰山东麓酿酒葡萄果栖产OTA真菌的分布
