CAJ | 학술논문

利用基质固相分散技术（MSPD），建立了超高效液相色谱-质谱检测器（MSD）同时分析牛奶中9种类固醇激素残留的方法。便携式 MSD的灵敏度和准确度优于紫外检测器；相比传统的质谱仪，MSD 不需质谱参数优化，操作简便，开机抽真空时间短（只要5 min），即开即用。分别考察了流动相比例、萃取溶剂和固相萃取小柱净化对MSD灵敏度和牛奶样品基质效应的影响。结果表明，MSD正离子模式对吸电子基团化合物的灵敏度更高，受外界条件影响大。经 MSPD净化后，9种类固醇激素的基质效应由84％~160％降低为80％~121％。方法学研究结果表明，9种类固醇激素的日内精密度和日间精密度分别为0.87％~1.78％和1.82％~3.79％，加标回收率为68.7％~94.7％，相对标准偏差（RSD）小于10％，方法检出限（LOD）为0.5~10μg／kg，定量限（LOQ）为2~20μg／kg。该方法适合日常大批量样品的检测。
이용기질고상분산기술（MSPD），건립료초고효액상색보-질보검측기（MSD）동시분석우내중9충류고순격소잔류적방법。편휴식 MSD적령민도화준학도우우자외검측기；상비전통적질보의，MSD 불수질보삼수우화，조작간편，개궤추진공시간단（지요5 min），즉개즉용。분별고찰료류동상비례、췌취용제화고상췌취소주정화대MSD령민도화우내양품기질효응적영향。결과표명，MSD정리자모식대흡전자기단화합물적령민도경고，수외계조건영향대。경 MSPD정화후，9충류고순격소적기질효응유84％~160％강저위80％~121％。방법학연구결과표명，9충류고순격소적일내정밀도화일간정밀도분별위0.87％~1.78％화1.82％~3.79％，가표회수솔위68.7％~94.7％，상대표준편차（RSD）소우10％，방법검출한（LOD）위0.5~10μg／kg，정량한（LOQ）위2~20μg／kg。해방법괄합일상대비량양품적검측。
An analytical method for the multiresidue determination of nine estrogenic steroids in milk was developed by modified matrix solid phase dispersion( MSPD)purification and ultra performance liquid chromatography( UPLC)with mass spectrometric detector( MSD). The sensitivity and accuracy of MSD were better than that of ultraviolet detector. In comparison with traditional mass spectrometry,the merits of MSD were simpler in operation and shorter in starting time(5 min). The results showed that the limits of detection of the compounds with nucleophilic substitution were high in positive ion mode of MSD and were easily affected by environmental conditions. The matrix effects of milk samples reduced from 84%-160% to 80%-121% after MSPD purification. The intraday precision and interday precision of the nine estro-genic steroids were 0. 87%-1. 78% and 1. 82%-3. 79%,respectively. The average recoveries were 68. 7%-94. 7%,and the relative standard deviations( RSDs)were less than 10%. The lim-its of detection( LODs)were 0. 5-10 μg/kg. The limits of quantification( LOQ)were 2-20μg/kg.