CAJ | 학술논문

利用免疫亲和萃取结合超高效液相色谱-串联四极杆质谱技术（UPLC-MS/MS）建立了乳及乳制品中黄曲霉毒素M1和M2的提取、分离、确证与定量方法。乙腈和水提取样品中的黄曲霉毒素，乙腈二次去蛋白后用免疫亲和柱净化，采用Waters Acquity UPLC R HSS T3（2.1×100 mm，1.7μm）色谱柱实现分离，多反应监测（MRM）模式下以外标法定量。结果表明：黄曲霉毒素M1和M2在0.1μg/L~50μg/L范围内线性关系良好（r﹥0.9985）；检出限为0.029μg/L~0.047μg/L（S/N=3）；2种黄曲霉毒素各添加水平在鲜牛奶、奶粉和奶油中的回收率为在69.56%~88.43%之间；相对标准偏差为3.69%~8.74%。
이용면역친화췌취결합초고효액상색보-천련사겁간질보기술（UPLC-MS/MS）건립료유급유제품중황곡매독소M1화M2적제취、분리、학증여정량방법。을정화수제취양품중적황곡매독소，을정이차거단백후용면역친화주정화，채용Waters Acquity UPLC R HSS T3（2.1×100 mm，1.7μm）색보주실현분리，다반응감측（MRM）모식하이외표법정량。결과표명：황곡매독소M1화M2재0.1μg/L~50μg/L범위내선성관계량호（r﹥0.9985）；검출한위0.029μg/L~0.047μg/L（S/N=3）；2충황곡매독소각첨가수평재선우내、내분화내유중적회수솔위재69.56%~88.43%지간；상대표준편차위3.69%~8.74%。
A method for the determination of 2 aflatoxins (M1,M2) in milk and dairy products by immunoaffinity extraction coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/M S) was developed. Aflatoxins in samples were extracted into acetonitrile/water system and deproteinized by adding additional acetonitrile, followed by stepwise purification using an immunoaffinity column. The target compounds were then eluted with methanol. With the gradient elution using a binary mobile phase containing of 0.1%formic acid solution and methanol/acetonitrile, the two aflatoxins were separated on a Waters Acquity UPLC R HSS T3 column (2.1 ×100 mm,1.7 μm particle size), followed by positive electrospray ionization and multi reaction monitoring provided by a triple-quadrupole tandem mass spectrometer,and quantified by external reference method. The calibration curve was linear over the concentration range of 0.1μg/L-50μg/L (r﹥0.998 5) and the detection limits of two aflatoxins were 0.029μg/L-0.047μg/L. The recoveries from milk, milk powder and cream were generally between 69.56%and 88.43%and the relative standard deviations were 3.69%-8.74%.