首页|特殊膳食食品中生物素含量测定方法研究

特殊膳食食品中生物素含量测定方法研究

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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0.22 μm滤膜,经Kinetex RR-C18(100 mm×2.1 mm,2.6 μm)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0.003 μg/g,定量限为0.01 μg/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.
Determination of Biotin in Special Dietary Foods
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 0.22 μm filter membrane,then was separated with Kinetex RR-C18(100 mm×2.1 mm,2.6 μm)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 0.003 μg/g,and the limit of quantitation was 0.01 μg/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.

biotinspecial dietary foodultra performance liquid chromatography-tandem mass spectrometry

贾静、常金良、杜凯、王立波、张李严、常梦蝶

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东营市工业产品检验与计量检定中心,山东东营 257091

东营市食品药品检验研究院,山东东营 257091

生物素 特殊膳食食品 超高效液相串联三重四极杆质谱法

东营市科技创新重大专项(科技发展指导计划)山东省市场监督管理局科研项目

2023ZDJH98sdscjgj2024zh03

2024

食品与药品
山东省生物药物研究院

食品与药品

CSTPCD
影响因子:0.537
ISSN:1672-979X
年,卷(期):2024.26(5)
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