CAJ | 학술논문

目的建立并优化高压液相色谱-串联质谱法快速检测奶粉中双氰胺残留的方法.方法奶粉样品经1%三氯乙酸溶液沉淀蛋白后,通过 Sep-pak AC-2离子交换固相萃取柱净化样品提取液,去除奶粉中其他复杂基质的干扰,浓缩后用初始流动相复溶、过膜.采用电喷雾正离子电离(ESI+)模式和多反应监测(MRM)扫描模式,通过 Acquity BEH Amide(3.0 mm×150 mm,1.7μm)色谱柱分离检测双氰胺目标化合物,同位素15N4-双氰胺稀释法定量.结果该方法在50~1200μg/kg 范围内线性良好,相关系数 r>0.998,在三种不同基质样品中的最低检测限与最低定量限分别为2.5μg/kg 和8μg/kg,加标回收率为93.4%~112.3%,相对标准偏差均<10.3%.结论该方法简便、灵敏、精确,不仅筛选优化了液相、质谱条件参数,同时优化了奶粉样品的前处理方法,适用于奶粉中双氰胺残留的检测.
목적건립병우화고압액상색보-천련질보법쾌속검측내분중쌍청알잔류적방법.방법내분양품경1%삼록을산용액침정단백후,통과 Sep-pak AC-2리자교환고상췌취주정화양품제취액,거제내분중기타복잡기질적간우,농축후용초시류동상복용、과막.채용전분무정리자전리(ESI+)모식화다반응감측(MRM)소묘모식,통과 Acquity BEH Amide(3.0 mm×150 mm,1.7μm)색보주분리검측쌍청알목표화합물,동위소15N4-쌍청알희석법정량.결과해방법재50~1200μg/kg 범위내선성량호,상관계수 r>0.998,재삼충불동기질양품중적최저검측한여최저정량한분별위2.5μg/kg 화8μg/kg,가표회수솔위93.4%~112.3%,상대표준편차균<10.3%.결론해방법간편、령민、정학,불부사선우화료액상、질보조건삼수,동시우화료내분양품적전처리방법,괄용우내분중쌍청알잔류적검측.
@@@@Objective To establish a rapid analytical method to determine the residues of dicyandiamide in milk powder. Methods After precipitating proteins of the milk powder sample by 1% trichloroacetic acid solution, the sample extract was purified by Sep-pak AC-2 ion exchange solid phase extraction column, which could remove the interference of complex matrix in the milk powder. Then it was concentrated and reconsti-tuted by the initial mobile phase, and went through the film. The dicyandiamide target compounds were sepa-rated by Acquity BEH Amide (3.0 mm×150 mm, 1.7 μm) column and were detected by liquid chromatogra-phy-tandem mass spectrometry (LC-MS) with electrospray ionization (ESI) in multiple reaction monitoring method (MRM). Accurate determination was achieved by using isotope 15N4-dicyandiamide as internal standard. Results The method showed a good linearity over the range of 50~1200 μg/kg with r>0.998 and the lowest detection limit and the lower limit of quantification in three different matrix samples were 2.5 μg/kg and 8μg/kg. The mean recoveries ranged from 93.4% to 112.3%. The relative standard deviation was less than 10.3%.Conclusion This method is simple, sensitive and accurate, and can not only optimize the parameters of the liquid phase and the conditions of mass spectrometry, but also optimize the pre-treatment methods of the milk powder sample. It can be applied to detect the residues of dicyandiamide in milk powder.