CAJ | 학술논문

建立了液相色谱_串联质谱法( LC_MS/MS)同时测定人工模拟猪胃和小肠消化液中黄曲霉毒素B1( AFB1)、脱氧雪腐镰刀菌烯醇( DON)和玉米赤霉烯酮( ZEA)的快速、灵敏方法,并将此方法应用于霉菌毒素吸附剂吸附率体外法评价。通过模拟猪的消化道对饲料基质进行体外消化获得猪胃和小肠消化液,分别向其中按一定比例添加霉菌毒素吸附剂和3种霉菌毒素,孵育、离心后,经进样液10倍稀释后测定。采用反相C18色谱柱分离,以0.2 mmol/L乙酸铵溶液和0.1%甲酸_甲醇溶液作为流动相,梯度洗脱,多反应监测离子模式( MRM)检测,同位素内标法定量。在优化条件下,对AFB1, DON和ZEA在人工猪胃和小肠消化液中的定量限分别是1,50,40μg/L和0.3,50,20μg/L,相对偏差(RSD)<5.0%。并且,在39℃±0.5℃,10 h内测定结果稳定,能够满足霉菌毒素吸附剂吸附率的测定。采用本方法对市售8种蒙脱石类吸附剂和5种酵母细胞壁类吸附剂进行吸附率评价。
건립료액상색보_천련질보법( LC_MS/MS)동시측정인공모의저위화소장소화액중황곡매독소B1( AFB1)、탈양설부렴도균희순( DON)화옥미적매희동( ZEA)적쾌속、령민방법,병장차방법응용우매균독소흡부제흡부솔체외법평개。통과모의저적소화도대사료기질진행체외소화획득저위화소장소화액,분별향기중안일정비례첨가매균독소흡부제화3충매균독소,부육、리심후,경진양액10배희석후측정。채용반상C18색보주분리,이0.2 mmol/L을산안용액화0.1%갑산_갑순용액작위류동상,제도세탈,다반응감측리자모식( MRM)검측,동위소내표법정량。재우화조건하,대AFB1, DON화ZEA재인공저위화소장소화액중적정량한분별시1,50,40μg/L화0.3,50,20μg/L,상대편차(RSD)<5.0%。병차,재39℃±0.5℃,10 h내측정결과은정,능구만족매균독소흡부제흡부솔적측정。채용본방법대시수8충몽탈석류흡부제화5충효모세포벽류흡부제진행흡부솔평개。
A rapid liquid chromatography_tandem mass spectrometric ( LC_MS/MS) method was developed for the determination of aflatoxin B1(AFB1), Deoxynivalenol (DON), Zearalenone (ZEA) in artificial porcine gastrointestinal digested juices, as pigs reacted most sensitively to these mycotoxins. The formula feed was digested by artificial gastric and intestinal juices respectively, then the mycotoxins and adsorbent were added in ratio. After incubation and centrifugation, the supernatant was diluted 10_folds by injection solution and analyzed by LC_MS/MS. The 3 analytes were separated on a reversed phase C18 column using a gradient elution program of aqueous solution containing 0 . 2 mmol/L ammonium acetate and 0 . 1% formic acid methanol. Qualitative analysis was performed using multiple_reaction monitoring ( MRM ) , and quantitative analysis was by internal standard method. Under optimum conditions, the limit of quantitation ( LOQ ) of AFB1 , DON, ZEA was 1, 50, 40 and 0. 3, 50, 20 μg/L in artificial gastric and intestinal digested juices respectively, and the relative standard deviations (RSDs) were below 5. 0%. Then, the thermal stability was studied by incubating the analytes at 39 ℃±0. 5 ℃ for 1, 2, 5 and 10 h, and the results showed 3 analytes were stable under the conditions. Furthermore, the method was applied to evaluate the binding efficacy of 8 mineral benders and 5 organic adsorbents. The adsorbents demonstrated binding efficacy of 85. 1%-96. 5%, 8 . 1%-14 . 7%, 13 . 7%-30 . 0% and 7 . 4%-16 . 6%, 6 . 7%-16 . 2%, 18 . 6%-39 . 0% in gastric digested juice, and 76. 2%-93. 0%, 12. 3%-31. 3%, 0%-23. 2% and 8. 6%-13. 4%, 3. 8%-23. 5%, 24. 9%-34. 8% in intestinal digested juice for these 3 mycotoxins, respectively, with 2 kinds of adsorbents.