食品研究与开发
食品研究與開髮
식품연구여개발
FOOD RESEARCH AND CEVELOPMENT
2014年
4期
82-86
,共5页
李佳峻%杨春林%胡强%吴蔚%吕小艇
李佳峻%楊春林%鬍彊%吳蔚%呂小艇
리가준%양춘림%호강%오위%려소정
超高效液相色谱-串联质谱%乳及乳制品%黄曲霉毒素%免疫亲和柱净化
超高效液相色譜-串聯質譜%乳及乳製品%黃麯黴毒素%免疫親和柱淨化
초고효액상색보-천련질보%유급유제품%황곡매독소%면역친화주정화
UPLC-MS/MS%fermented condiment%aflatoxins%immunoaffinity column clean-up
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%。
利用免疫親和萃取結閤超高效液相色譜-串聯四極桿質譜技術(UPLC-MS/MS)建立瞭乳及乳製品中黃麯黴毒素M1和M2的提取、分離、確證與定量方法。乙腈和水提取樣品中的黃麯黴毒素,乙腈二次去蛋白後用免疫親和柱淨化,採用Waters Acquity UPLC R HSS T3(2.1×100 mm,1.7μm)色譜柱實現分離,多反應鑑測(MRM)模式下以外標法定量。結果錶明:黃麯黴毒素M1和M2在0.1μg/L~50μg/L範圍內線性關繫良好(r﹥0.9985);檢齣限為0.029μg/L~0.047μg/L(S/N=3);2種黃麯黴毒素各添加水平在鮮牛奶、奶粉和奶油中的迴收率為在69.56%~88.43%之間;相對標準偏差為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%.