Wei Yunji, Feng Min, Zhu Zhenyi, He Jian, Shen Jinrong, He Zhenghe, Qin Xian, Zhou Liying
State Key Laboratory of Feed Safety Testing(Huai'an), Huai'an Entry-Exit Inspection and Quarantine Bureau, Huai'an 223001, China.
Kunshan Entry-Exit Inspection and Quarantine Bureau, Kunshan 215300, China.
Se Pu. 2017 Aug 8;35(8):891-896. doi: 10.3724/SP.J.1123.2017.03042.
A high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the simultaneous determination of 11 mycotoxins in feeds. The samples were extracted with acetonitrile, then cleaned up by multifunctional purification column filler and PRIME HLB solid phase extraction column. The 11 mycotoxins were separated on an Agilent Zorbax SB-C18 column (150 mm×2.1 mm, 3.5 μ m) with gradient elution program, and methanol-5 mmol/L ammonium acetate solution containing 0.1%(v/v) formic acid were used as mobile phases. The target compounds were detected under electrospray ionization (ESI) both in positive and negative modes with multiple reaction monitoring mode, and quantified by internal standard method. The results indicated that the 11 mycotoxins showed good linear relationships in their respective linear ranges, and the correlation coefficients were greater than 0.99. The limits of quantification (LOQs) were between 2.0 and 50.0 μ g/kg. The average recoveries were between 79.3% and 101.6% at three spiked levels (1, 2 and 5 times LOQs) with relative standard deviations (RSDs) of 5.9%-13.2% (=5). The method is simple, rapid, sensitive, and can be used for the analysis of the 11 mycotoxins in feeds.
建立了一种高效液相色谱 - 串联质谱（HPLC-MS/MS）法同时测定饲料中的11种霉菌毒素。样品用乙腈提取，然后通过多功能净化柱填料和PRIME HLB固相萃取柱进行净化。11种霉菌毒素在Agilent Zorbax SB-C18柱（150 mm×2.1 mm，3.5μm）上采用梯度洗脱程序进行分离，以含0.1%（v/v）甲酸的甲醇 - 5 mmol/L醋酸铵溶液作为流动相。目标化合物在电喷雾电离（ESI）正、负离子模式下采用多反应监测模式进行检测，并以内标法进行定量。结果表明，11种霉菌毒素在各自的线性范围内呈现良好的线性关系，相关系数大于0.99。定量限（LOQs）在2.0至50.0μg/kg之间。在三个加标水平（1、2和5倍LOQs）下的平均回收率在79.3%至101.6%之间，相对标准偏差（RSDs）为5.9% - 13.2%（n = 5）。该方法简便、快速、灵敏，可用于饲料中11种霉菌毒素的分析。
