CAJ | 학술논문

建立了同时检测玉米、豆粕等饲料原料中脱氧雪腐镰刀菌烯醇等26种霉菌毒素的液相色谱-串联质谱(LC-MS/MS)方法。玉米和豆粕样品经乙腈-水-甲酸(84：15.9：0.1, V/V)超声提取1 h,取1 mL上清液经Mycospin 400多功能净化柱净化,浓缩干燥,0.25 mL水-甲醇-甲酸(95：4.9：0.1, V/V)复溶,上机测定。采用反相C18色谱柱分离,以0.1%甲酸-水和0.1%甲酸-甲醇溶液作为流动相进行梯度洗脱,采用多反应监测离子模式进行定性分析。基质效应考察发现,样品提取液经Mycospin 400多功能净化柱净化后,大部分毒素仍有较强的基质效应。因此,采用基质匹配标准曲线外标法进行定量分析。在高、中、低3种添加浓度水平下,26种霉菌毒素的平均回收率为61.9%~119.5%,相对标准偏差介于0.8%~18.6%之间。针对不同目标物,本方法的定量限为0.5~25μg/kg。
건립료동시검측옥미、두박등사료원료중탈양설부렴도균희순등26충매균독소적액상색보-천련질보(LC-MS/MS)방법。옥미화두박양품경을정-수-갑산(84：15.9：0.1, V/V)초성제취1 h,취1 mL상청액경Mycospin 400다공능정화주정화,농축간조,0.25 mL수-갑순-갑산(95：4.9：0.1, V/V)복용,상궤측정。채용반상C18색보주분리,이0.1%갑산-수화0.1%갑산-갑순용액작위류동상진행제도세탈,채용다반응감측리자모식진행정성분석。기질효응고찰발현,양품제취액경Mycospin 400다공능정화주정화후,대부분독소잉유교강적기질효응。인차,채용기질필배표준곡선외표법진행정량분석。재고、중、저3충첨가농도수평하,26충매균독소적평균회수솔위61.9%~119.5%,상대표준편차개우0.8%~18.6%지간。침대불동목표물,본방법적정량한위0.5~25μg/kg。
A rapid high-throughput method for the determination of 26 mycotoxins involving multifunctional cleanup column coupled with liquid chromatography-tandem mass spectrometry ( LC-MS/MS) was developed and validated for the determination in feedstuffs. The feedstuff samples were extracted by ultrasonic treatment for 1 hour and the extraction solvent was acetonitrile/water/formic acid (84:15. 9:0. 1, V/V). 1 mL of the supernatant layer was purified by a commercial Mycospin 400 multifunctional cleanup column, then dried and re-dissolved by 0. 25 mL water/methanol/formic acid (95:4. 9:0. 1, V/V) in a vial for injection into the LC-MS/MS system. Chromatographic analyses were carried out on a reversed phase C18 column and using a gradient elution with 0. 1% formic acid aqueous solution and 0. 1% formic acid methanol solution. The mass spectrometer was operated in a multiple reaction monitoring ( MRM) mode that selected one precursor ion and two product ions for each target compound. Validation studies were carried out in maize and soybean meal as representative matrixes. The most target compounds had different level of matrix effects. So, matrix-matched calibration was adopted for quantification. Mean recoveries from spiked samples at three levels ranged from 61 . 9% to 119 . 5% with relative standard deviations of 0 . 8%-18 . 6%. Limits of quantification ranged from 0. 5 μg/kg to 25 μg/kg.