反相高效液相色谱法测定牦牛乳中的 B 族维生素含量

董爱军; 杨鑫; 张英春; 张华; 井晶

doi:10.13386/j.issn1002-0306.2017.03.052

反相高效液相色谱法测定牦牛乳中的 B 族维生素含量

哈尔滨工业大学化工与化学学院

详细信息

作者简介:
董爱军(1969-),女,硕士,副教授,研究方向:食品质量与安全,E-mail:daj@hit.edu.cn。;

杨鑫(1977-),男,博士,教授,研究方向:食品质量与安全,E-mail:yangxin@hit.edu.cn。;

中图分类号: TS252.7;O657.72
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出版历程
- 收稿日期: 2016-07-27

Determination of vitamin B in yak milk by reversed phase high performance liquid chromatography method

School of Chemistry and Chemical Engineering,Harbin Institute of Technology

摘要

摘要: 建立了同时测定牦牛乳中维生素B₁、B₂、B₃、B₆、B₁2的高效液相色谱法,样品经离心脱脂,高氯酸除蛋白后,采用反相色谱柱分离,DAD检测器检测,外标法定量。色谱柱为C₁8柱（25 mm×4.6 mm,i.d.5μm）,流动相为0.023 mol/L H₃PO₄溶液（pH3.54）和甲醇,采用梯度洗脱,流速为0.5 mL/min,柱温25℃,检测波长270 nm。结果表明:维生素B₂、B₃在0.1⁵0.0 mg/L,维生素B₁、B₆、B₁2在0.5²50.0 mg/L质量浓度范围内呈现良好的线性关系,相关系数均为0.999。5种B族维生素的平均回收率为90.6%⁹8.4%,相对标准偏差（RSDs）为2.0%⁴.3%,在牦牛乳中的检出限为0.01⁰.09 mg/L,定量下限为0.03⁰.29 mg/L。本方法样品处理简单,分析速度快,准确度和精密度高,能够满足快速分析需要。
- 牦牛乳 /
- 水溶性维生素 /
- 维生素B /
- 高效液相色谱
Abstract: A method was developed for the determination of vitamin B_1,B_2,B_3,B_6,B_12 in yak milk by reversed phase high performance liquid chromatography method. After derosination by centrifugation and deproteinization with perchloric acid,the sample was separated on a C_18 column( 250 mm × 4.6 mm,i.d.5 μm) at 25 ℃. A gradient programme was carried out using 0.023 mol/L H_3PO_4( pH3.54) and methyl alcohol as elution solvent at a flow rate of 0.5 mL/min. The response signal was detected at 270 nm.The results showed that vitamin B_1,B_2,B_3,B_6,B_12 could be separated within 20 min.The calibration curves were linear in the ranges of 0.1 ~ 50.0 mg/L for vitamin B_2,B_3,and 0.5~250.0 mg/L for vitamin B_1,B_6,B_12 with correlation coefficient of 0.999. The spiked recoveries of vitamin B in yak milk were in the range of 90.6% ~ 98.4% with the relative standard deviations( RSDs) of 2.0% ~4.3%. The limits of detection( LODs) of five vitamin B in yak milk were in the range of 0.01~0.09 mg/L,the limits of quantitation( LOQs) were 0.03 ~ 0.29 mg/L. The developed method was sensitive and precise,which could meet the demands of rapid analysis.
- yak milk /
- water-soluble vitamins /
- vitamin B /
- high performance liquid chromatography

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