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应用SPE柱净化HPLC/UV法测定乳制品及其原料中的硫氰酸盐

陶保华 赖世云 傅士姗 蔡增轩 张京顺 董亦波 任一平

分析测试学报2012,Vol.31Issue(6):686-690,5.
分析测试学报2012,Vol.31Issue(6):686-690,5.DOI:10.3969/j.issn.1004-4957.2012.06.010

应用SPE柱净化HPLC/UV法测定乳制品及其原料中的硫氰酸盐

Determination of Thiocyanate in Milk Products and Raw Materials by HPLC/UV with SPE Extraction

陶保华 1赖世云 1傅士姗 1蔡增轩 2张京顺 3董亦波 1任一平2

作者信息

  • 1. 贝因美研究院,浙江 杭州 310057
  • 2. 浙江省疾病预防控制中心,浙江 杭州 310051
  • 3. 浙江大学 生物系统工程与食品科学学院,浙江 杭州 310029
  • 折叠

摘要

Abstract

A high performance liquid chromatography with tunable ultraviolet method ( HPLC - UV) was developed for the quantification of thiocyanate in milk products and raw materials. Samples were purified and extracted by Oasis WAX SPEs followed by protein precipitation with acetic acid. The purified solution was separated on a symmetry Clg column using methanol - phosphatic solution (containing ion pair reagent) as mobile phase, and analyzed by the internal standard method at a detection wavelength of 231 nm. Under the optimal conditions, the linear range for thiocyanate was in the range of 0. 2 - 50 mg/L with correlation coefficient more than 0. 999. The limit of detection for thiocyanate was 0. 05 mg/kg, and the limit of quantitation (LOQ) was 0. 15 mg/kg. The recoveries at spiked concentration levels of 1, 5, 25 mg/kg were in the range of 77% - 104% . With the advantages of excellent reproducibility, high sensitivity and good practicability, this method could be used as a routine detection in practice.

关键词

硫氰酸盐/SPE净化/高效液相色谱/紫外检测/乳制品

Key words

thiocyanate/ SPE extract/ HPLC/ ultraviolet detection/ milk product

分类

化学化工

引用本文复制引用

陶保华,赖世云,傅士姗,蔡增轩,张京顺,董亦波,任一平..应用SPE柱净化HPLC/UV法测定乳制品及其原料中的硫氰酸盐[J].分析测试学报,2012,31(6):686-690,5.

分析测试学报

OA北大核心CSCDCSTPCD

1004-4957

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