HPLC-MS/MS测定八宝粥中8种霉菌毒素

Determination of 8 Mycotoxins in Eight-treasure Porridge by HPLC-MS/MS

建立了测定八宝粥中黄曲霉毒素B_1、B_2、G_1、G_2,T-2毒素,赭曲霉毒素A,玉米赤霉烯酮和杂色曲霉素8种霉菌毒素的高效液相色谱串联质谱(HPLC-MS/MS)法。样品经乙腈-水(88:12,V/V)超声提取、离心后,用多功能净化柱净化,以乙腈和5 mmol/L甲酸铵水溶液(含0.1%甲酸)为流动相梯度洗脱,经ZORBAX Eclipse Plus C_(18)色谱柱(2.1 mm×100 mm,1.8μm)分离,多反应监测(MRM)正离子模式进行检测,外标法定量。在0.5~50.0 ng/mL的浓度范围内,8种霉菌毒素均具有良好的线性关系(r≥0.999 6)。此方法的检出限为0.06~0.18μg/kg,平均回收率为73.5%~97.4%,RSD为4.6%~8.2%(n=7)。该方法简便、准确、灵敏,适用于八宝粥中黄曲霉毒素B_1、B_2、G_1、G_2,T-2毒素,赭曲霉毒素A,玉米赤霉烯酮和杂色曲霉素的同时检测。

A method was developed for the determination of 8 mycotoxins, including aflatoxin B1, B2, G1, G2, T-2, ochratoxin A（OTA）, zearalenone（ZEN） and sterigmatocystin（STC） in eight-treasure porridge by high performance liquid chromatography tandem mass spectrometry（HPLC-MS/MS）. The samples were extracted ultrasonically by acetonitrile-water（88：12, V/V）, and then centrifuged. After the supernatant liquid was purified through multifunctional clean-up column, the 8 mycotoxins were separated by ZORBAX Eclipse Plus C（18） column（2.1 mm×100 mm, 1.8 μm） with acetonitrile and 5 mmol/L ammonium acetate aqueous solution（containing 0.1% formic acid） as mobile phase for gradient elution, and determined by HPLC-MS/MS with positive ion mode of electrospray ionization under multiple reaction monitoring（MRM）, quantified by external standard method. In the range of 0.5-50.0 ng/mL, the calibration curves showed good linearity for 8 mycotoxins with good correlative coefficients（r≥0.999 6）. The limits of detection were 0.06-0.18 μg/kg. The average recoveries of 8 mycotoxins in spiked samples were 73.5%-97.4% with the relative standard deviation（RSD） of 4.6%-8.2%（n=7）. The method is easy, accurate and sensitive, which can be applied in the simultaneous determination of aflatoxin B1, B2, G1, G2, T-2, OTA, ZEN and STC in eight-treasure porridge.