色谱2011，Vol.29Issue(6)：517-522,6.DOI:10.3724/SP.J.1123.2011.00517
液相色谱-三重串联四极杆质谱测定粮油中的黄曲霉毒素
Determination of aflatoxins in cereals and oils by liquid chromatography-triple quadrupole tandem mass spectrometry
摘要
Abstract
The high performance liquid chromatography ( HPLC) -triple quadrupole tandem mass spectrometry was applied for the determination of the aflatoxins: B, (AFB,) , B2( AFB2) , G, (AFG1) and G2( AFG2), in cereals and oils. The samples were first extracted by ultrasonic method. The optimized conditions of ultrasonic extraction were as follows: temperature of 50 ℃, extraction time of 3 min, methanol-water (containing 40 g/L NaCl) (80=20, v/v) solution as the medium and a ratio of sample to solvent of 1: 3 (g: mL). The extracts were then purified using an immunoaffinity column. The separation was performed on a Cl8 column with mobile phases of 10 mmol/L ammonium acetate and methanol in gradient elution. The sensitive detection of the four AFT compounds by electrospray ionization mass spectrometry (ESI-MS) was carried out in selected reaction monitoring (SRM) mode with aflatoxin Ml (AFM, ) as the internal standard. Under the optimized conditions, the limits of detection of AFB,, AFB2, AFG, and AFG2 were 0.002, 0.004, 0.004 and 0.012 |xg/kg, respectively. The recoveries of aflatoxins in different spiked cereals and oils were in the range from 87% to 111%. The intra-day and inter-day precisions were not more than 6. 7% and 5. 6%, respectively. In comparison with the external standard method, this method can effectively inhibit the matrix effects, and greatly improve the accuracy.关键词
超声提取/液相色谱-质谱/内标校正/免疫亲和/黄曲霉毒素/粮油Key words
ultrasonic extraction/ liquid chromatography-mass spectrometry (LC-MS) / internal standard calibration/ immunoaffinity/ aflatoxin (AFT)/ cereals and oils分类
化学化工引用本文复制引用
王秀嫔,李英,姜俊,李培武,杨扬,张文,张奇,范素芳,喻理,王琳,陈小媚..液相色谱-三重串联四极杆质谱测定粮油中的黄曲霉毒素[J].色谱,2011,29(6):517-522,6.基金项目
农业部"948"重点项目(2010-G1,2009-Z46)、国家科技支撑计划项目(2010BAD01B07,2011BAD02D02)、湖北省自然科学基金项目(2010CDB10602)、国家油菜现代产业技术体系项目(nycytx-005)、国家自然科学基金项目(31000787)和中国农业科学院所长基金项目(1610172010004). （2010-G1,2009-Z46）
