特殊膳食食品中生物素含量测定方法研究  

Determination of Biotin in Special Dietary Foods

作　　者：贾静 常金良 杜凯 王立波 张李严 常梦蝶 JIA Jing;CHANG Jin-liang;DU Kai;WANG Li-bo;ZHANG Li-yan;CHANG Meng-die(Dongying Center for Industrial Products Inspection and Metrological Verification,Dongying 257091,China;Dongying Institute for Food and Drug Control,Dongying 257091,China)

机构地区：[1]东营市工业产品检验与计量检定中心,山东东营257091 [2]东营市食品药品检验研究院,山东东营257091

出　　处：《食品与药品》2024年第5期389-393,共5页Food and Drug

基　　金：东营市科技创新重大专项(科技发展指导计划)(编号:2023ZDJH98);山东省市场监督管理局科研项目(编号:sdscjgj2024zh03)。

摘　　要：目的建立超高效液相串联三重四极杆质谱法(UPLC-MS/MS)测定特殊膳食食品中生物素含量的方法。方法试样中加入内标物,采用40℃温水提取,振荡混匀后超声提取,冷却后用高氯酸调节pH至1.6±0.2,离心,上清用氢氧化钠溶液调节pH至4.5±0.2,再次离心,上清过0.22μm滤膜,经Kinetex RR-C_(18)(100 mm×2.1mm,2.6μm)色谱柱分离,以0.1%甲酸水溶液-乙腈为流动相,以内标法定量。结果生物素在1~50 ng/ml范围内具有良好的线性关系(r>0.999),方法检出限为0.003μg/g,定量限为0.01μg/g。在10 h内样品提取液中生物素含量稳定,RSD为5.87%。在5,15,30 ng/ml加标水平下的平均回收率为90.7%~116.9%,RSD为1.71%~4.42%(n=6)。结论此法检测速度快、灵敏度高、重复性好,适用于特殊膳食食品中生物素含量的快速及准确测定。Objective To establish a method for the simultaneous determination of biotin in special dietary foods by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were added internal standard substance and warm water of 40℃,and were ultrasonically extracted after oscillation and mixing,then cooled to room temperature.The pH values of the samples were then adjusted to 1.6±0.2 with perchloric acid.After centrifugation,the pH values of the supernatant were adjusted to 4.5±0.2 by sodium hydroxide.After being centrifuged again,the supernatant was filtered by 0.22μm filter membrane,then was separated with Kinetex RR-C_(18)(100 mm×2.1 mm,2.6μm)column,using 0.1%formic acid aqueous solution-acetonitrile as mobile phase.The quantitative analysis was performed through internal standard method.Results The biotin had good linear relationship in the range of 1-50 ng/ml(r>0.999).The limit of detection was 0.003μg/g,and the limit of quantitation was 0.01μg/g.The content of biotin in sample extract solution was stable within 10 h,and the RSD was 5.87%.The average recoveries at the spiked levels of 5,15,30 ng/ml were 90.7%-116.9%,with RSDs of 1.71%-4.42%(n=6).Conclusion This method has fast detection speed,high sensitivity and good repeatability,and is suitable for rapid detection and confirmatory analysis of biotin in special dietary foods.

关 键 词：生物素 特殊膳食食品 超高效液相串联三重四极杆质谱法 

分 类 号：O657[理学—分析化学] TS218[理学—化学]