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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 establish a method for the determination of aflatoxin B1, zearalenone and ochratoxin in corn by high performance liquid chromatography. Methods After the corn samples were extracted with aqueous methanol (V / V = 80:20), the extract was used as dispersant and chloroform as extractant. Aflatoxin B1, zearalenone and ochratoxin were dispersed by liquid and liquid Microextraction was used to enrich and purify the samples. C18 column was used as the separation column, acetonitrile and 1% acetic acid aqueous solution were used as the mobile phase gradient elution, and the three kinds of toxins were detected by variable wavelength method. Results The linear ranges of aflatoxin B1, zearalenone and ochratoxin were 1.00-100 ng / ml (r = 0.9985), 5.00-1000 ng / ml (r = 0.999 6) and 1.00 ~ The detection limits were 0.1,1.0 and 0.3 μg / kg, respectively. The average recoveries ranged from 82.5% to 99.3% with RSD <10% (n = 6). Conclusion The method is rapid, sensitive, accurate and reliable and is suitable for simultaneous determination of aflatoxin B1, zearalenone and ochratoxin in maize samples.