药食两用类食品中赭曲霉毒素A的高效液相色谱-荧光检测方法  

Determination of Ochratoxin A in Edible and Medicinal Foods by HPLC-Fluorescence Technology

作　　者：傅武胜[1,2] 邱文倩[1] 郑奎城[1] 吕华东[1] 郭斌[3] 严小波[4] 

机构地区：[1]福建省疾病预防控制中心,福建福州350001 [2]福建医科大学福建省疾病预防控制中心教学基地,福建福州350001 [3]福建中医药大学,福建福州350001 [4]福州大学化学化工学院,福建福州350001

出　　处：《食品科学》2011年第14期298-302,共5页Food Science

基　　金：福建省科技计划重点项目(2008Y0029)

摘　　要：目的:采用免疫亲和净化和高效液相色谱技术,建立淀粉、糖类药食两用食品中赭曲霉毒素A的测定方法。方法:样品粉末经甲醇-水(8:2,V/V)涡旋、超声及振摇提取,提取液以磷酸盐缓冲液稀释后,用商品免疫亲和柱净化,含有赭曲霉毒素A的甲醇洗脱液用高效液相色谱技术分析,C18反相色谱柱分离,荧光检测器测定。结果:赭曲霉毒素A的最低检出浓度为1.0μg/kg(RSN=3);在0.5～100ng/mL范围内,峰面积与质量浓度呈线性关系(r=0.9995);以不含赭曲霉毒素A的太子参、莲子、薏苡、麦冬和龙眼肉为加标基质,加标水平为1～8μg/kg时,平均回收率在81.8%～107%之间,RSD为1.66%～15.0%(n=3)。结论:免疫亲和柱能和高效液相色谱-荧光检测相结合取得较为满意的结果,准确度高、精密度好,满足欧盟对食品饲料中OTA检测方法的要求,适合于淀粉、糖类药食两用食品中赭曲霉毒素A的测定。Objective： To develop a method to determine ochratoxin A （OTA） in edible and medicinal foods using immunoaffinity column purification and high performance liquid chromatography （HPLC）. Methods： Powdered samples were extracted with methanol-water （8：2, V/V） sequentially by vortex mixing, ultrasonic treatment and shaking. The resulting extract was diluted with phosphate buffer solution, filtrated and cleaned up on immunoaffmity column （IAC） containing antibodies specific to OTA. The pooled eluate was separated on a C18 column （4.6 mm × 150 ram, 3 μ m） and detected by fluorescence detector （FLD）. Results： The limit of detection （LOD, RSN = 3） was 1,0 μ g/kg for OTA. An excellent linear relationship between peak area and OTA concentration was observed in the OTA concentration range of 0.5 - 100 ng/mL with correlation coefficient of 0.9995. The average recovery rates for OTA in prince ginseng root, lotus seed, coix seed, Radix Ophiopgonis, dried longan pulp and oriental water plantain rhizome spiked with OTA standard at a level of 1 - 8/a g/kg were varied from 81.8% - 107% with a relative standard deviation （RSD） of 1.66%- 15.0% （n = 3）. Conclusion： This method has the advantages of satisfactory results and high accuracy and precision and can meet the requirements of the Europe Union for the determination of OTA in food and feed, thus providing a suitable method for determining OTA edible and medicinal foods rich in starch or sugar.

关 键 词：药食两用食品 赭曲霉毒素A 免疫亲和净化 高效液相色谱法 

分 类 号：O656.31[理学—分析化学]