摘要
目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定牛乳基婴幼儿配方奶粉中的乳铁蛋白含量的分析方法。方法试样中的乳铁蛋白经尿素-碳酸氢铵缓冲液提取,二硫苏糖醇还原,碘乙酰胺烷基化,37℃酶解后,特征肽段用液相色谱-串联质谱正离子模式测定,内标法定量。结果乳铁蛋白在0.00080~0.16000 pmol/μL(相当于10~2000 mg/100 g)水平间线性关系良好,相关系数r=0.9997,定量限为0.0020 pmol/μL(相当于25 mg/100 g),加标回收率为89.71%~106.28%,相对标准偏差为2.96%~4.15%。结论该方法准确度好、特异性强、灵敏度高,可用于牛乳基婴幼儿配方奶粉中的乳铁蛋白含量的测定。
Objective To establish a method for the determination of lactoferrin in milk-based infant formula by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods Lactoferrin was extracted by urea-ammonium bicarbonate buffer,reduced with dithiothreitol,alkylated with iodoacetamide,digested at 37 ℃.Afterwards,the lactoferrin was quantified using the derived signature peptides using liquid chromatography-tandem mass spectrometry in positive ion mode with correction of isotope-labelling internal standard.Results The method showed a good linearity between 0.00080-0.16000 pmol/μL(correspond to 10-2000 mg/100 g) with the correlation coefficient r=0.9997.The limit of quantitation for the method was 0.0020 pmol/μL,which was equivalent to 25 mg/100 g.The recoveries ranged from 89.71% to 106.28%,and relative standard deviations varied from 2.96%-4.15%.Conclusion The proposed method has good accuracy and specificity,as well as high sensitivity,which can be used for the determination of lactoferrin in milk-based infant formula.
作者
赵飒
张晓梅
鲍蕾
魏帅
高瑞刚
马世波
李明哲
卜汉萍
何京澄
张鸿伟
梁成珠
ZHAO Sa;ZHANG Xiao-Mei;BAO Lei;WEI Shuai;GAO Rui-Gang;MA Shi-Bo;LI Ming-Zhe;BU Han-Ping;HE Jing-Cheng;ZHANG Hong-Wei;LIANG Cheng-Zhu(Technology Center of Qingdao Customs District,Qingdao 266114,China;NestléFood Safety Institute,NestléResearch&Development(China)Co.,Ltd.,Beijing 100015,China;Synutra Nutrition Foods Co.,Ltd.,Qingdao 266400,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第24期9326-9333,共8页
Journal of Food Safety and Quality
基金
国家重点研发计划项目(2017YFE0110800)
青岛海关科研项目(QK202101)。
