摘要
目的建立玉米中黄曲霉毒素B1、玉米赤霉烯酮和赭曲霉毒素的高效液相色谱测定法。方法玉米样品经甲醇水溶液(V/V=80∶20)提取后,以提取液为分散剂,三氯甲烷为萃取剂,黄曲霉毒素B1、玉米赤霉烯酮和赭曲霉毒素经液液分散式微萃取富集净化,以C18色谱柱为分离柱,以乙腈和1%乙酸水溶液为流动相梯度洗脱分离后,采用变波长的方法对三种毒素进行检测。结果黄曲霉毒素B1、玉米赤霉烯酮和赭曲霉毒素的线性范围分别为:1.00-100 ng/ml(r=0.998 5)、5.00-1 000 ng/ml(r=0.999 6)和1.00-100 ng/ml(r=0.999 3),检出限分别为:0.1、1.0和0.3μg/kg,平均加标回收率范围:82.5%-99.3%,RSD<10%(n=6)。结论该方法快速、灵敏、准确可靠,适用于玉米样品中黄曲霉毒素B1,玉米赤霉烯酮和赭曲霉毒素的同时检测。
Objective To develop a method for the simultaneous determination of aflatoxin B1(AFB1), zearalenone(ZEN) and ochratoxin A(OTA) in corn using high-performance liquid chromatography(HPLC) with fluorescence detector(FLD). Methods After extraction of the corn samples with a mixture of methanol-water(V∶V=80∶20), mycotoxins were rapidly partitioned into a small volume of chloroform by dispersive liquid-liquid microextraction. The three mycotoxins were simultaneously determined using HPLC-FLD under their best wavelength by means of changing of fluorescence excitation and emission wavelength and gradient eluted program. Results The linear ranges were 1.00-100 ng/ml for AFB1, 5.00-1 000 ng/ml for ZEN and 1.00-100 ng/ml for OTA, with the correlation coefficient(r) of 0.998 5, 0.999 6 and 0.999 3, respectively. Limits of detection(LODs) were 0.10,1.0 and 0.3 μg/kg, the mean recoveries were in the range of 82.5% to 99.3% with RSD 10%(n =6, independent analysis).Conclusion The proposed method is demonstrated to be simple, highly sensitivity, accurate, reliable, and is successfully applied to simultaneously analysis of AFB1, ZEN and OTA in real corn samples.
出处
《环境与健康杂志》
CAS
北大核心
2016年第7期633-636,共4页
Journal of Environment and Health