摘要
目的:建立了同时测定茶叶中脱氧雪腐镰刀菌烯醇、黄曲霉毒素B1、黄曲霉毒素B2、黄曲霉毒素G1、黄曲霉毒素G2、玉米赤霉烯酮等6种真菌毒素免疫亲和柱-高效液相色谱检测方法。方法:样品经粉碎,乙腈-水(体积比为86:14)超声提取,自制复合免疫亲和柱净化,Accurasil C18柱(4.6mm×250mm,5μm)色谱柱分离,甲醇-乙腈(体积比为1:1)和水为流动相梯度洗脱,二极管阵列检测器串联在线柱后光化学衍生装置和荧光检测器同时检测,外标法定量。结果:茶叶中的6种真菌毒素在各自浓度范围内线性关系良好,相关系数均大于0.999;3个不同添加水平的平均加标回收率为68.0%~88.3%,相对标准偏差(n=6)为2.6%~9.2%,检出限(S/N=3)为0.12~10.0μg/kg。结论:该方法简便、高效、抗基质干扰能力强,大大降低假阳性样品的检出率,可满足各种茶叶中6种真菌毒素同时检测的需求。
The samples of six mycotoxins(deoxynival enol(DON),AFB1、AFB2、AFG1、AFG2and zearalenone(ZEA))in tea were pounded,homogenized and extracted with acetonitrile-water(86:14,V/V),and purified by self-immunoaffinity column.Using accurasil C18 column(4.6mm×250mm,5μm)as separated column,with mixtures of methanol、acetonitrile and water as mobile phase for gradient elution,and using FLD and DAD for determination after post column photochemical derivatization.The results showed that linear relationship between values of peak area and mass concentration of the six mycotoxins were kept in definite ranges,and the correlation coefficient was greater than 0.999,with detection limits(3S/N)in the range of 0.12—10.0μg/kg.On the base of bland black tea,the average recoveries of three spiked levels were 68.0%—88.3%,with relative standard deviations of 2.6%—9.2%.This method is simple,efficient,and has a strong anti-matrix interference ability which can reduce the detection rate of false positive samples greatly.
作者
吴定芳
王磊
戴佩珍
何茫茫
Wu Dingfang;Wang Lei;Dai Peizhen;He Mangmang(Rui’an Food Inspection and Testing Center,Wenzhou 325204,China;Rui’an Tangxia People’s Hospital,Wenzhou 325204,China)
出处
《分析仪器》
CAS
2023年第1期32-38,共7页
Analytical Instrumentation
基金
温州市基础性科研项目(N20190019)。
关键词
高效液相色谱法
茶叶
真菌毒素
免疫亲和柱
光化学衍生
High performance liquid chromatography(HPLC)
Tea
Mycotoxins
Immunoaffinity column
Photochemical derivatization