高效液相色谱-三重四级杆质谱法同时测定大米中的伏马毒素B_1、B_2、B_3

Simultaneous determination of fumonisins B_1,B_2 and B_3 in rice by high-performance liquid chromatography-triple quadrupole mass spectrometry

目的建立高效液相色谱-三重四级杆质谱法同时测定大米中的伏马毒素B_1、B_2、B_3。方法大米样品经乙腈:水=50:50提取,以Multistep@211 Fum柱进行净化,将洗脱液氮吹至干,加1.0 ml 0.2%甲酸/乙腈=65:35溶解并定容,用LC-MS/MS检测。结果待测组分在5~800 ng/ml范围内呈现良好的线性关系,相关系数均大于0.9996,检测限介于0.045~0.10 ng/ml。以空白大米粉样品进行加标水平分别为20、100、400 ng/g的回收率实验,回收率在94.5%~110.5%之间。结论该方法快速、准确,适用于大米中伏马毒素的测定。

Objective To establish a method for simultaneous determination of fumonisins B1, B2 and B3 in rice by high-performance liquid chromatography coupled with triple quadrupole mass spectrometry （HPLC-TQMS）. Methods The fumonisins were extracted with 50% acetonitrile in a water bath, and purified by Multistep@211 Fum extraction cartridge. The eluate was concentrated to dryness, and dissolved with 1.0 ml 0.2% formic acid /acetonitrile=65：35, and then detected by HPLC-TQMS. Results Target compounds presented a good linear relationship in the range of 5-800 ng/ml. The correlation coefficients were larger than 0.9996 and the limits of detection were in the range of 0.045-0.10 ng/ml. The recoveries of standard addition for spiked samples in 20 ng/g,100 ng/g, and 400 ng/g were between 94.5%-110.5%. Conclusions The proposed method is rapid, accurate and suitable for determining fumonisins in rice.