色谱

色谱 ›› 2014, Vol. 32 ›› Issue (2): 174-178.DOI: 10.3724/SP.J.1123.2013.09047

• 技术与应用 • 上一篇    下一篇

微波灰化-液相色谱-电感耦合等离子体质谱联用测定干食用菌中的三价铬和六价铬

倪张林, 汤富彬, 屈明华, 莫润宏   

  1. 中国林业科学研究院亚热带林业研究所, 国家林业局经济林产品质量检验检测中心(杭州), 浙江 富阳 311400
  • 收稿日期:2013-09-29 修回日期:2013-11-27 出版日期:2014-02-08 发布日期:2014-01-25
  • 通讯作者: 汤富彬
  • 基金资助:

    国家林业公益性行业科研专项课题(201304705，201204414).

Determination of trivalent chromium and hexavalent chromium in dried edible fungi by microwave ashing-liquid chromatography with inductively coupled plasma mass spectrometry

NI Zhanglin, TANG Fubin, QU Minghua, MO Runhong   

  1. Research Institute of Subtropical Forestry, Chinese Academy of Forestry; Quality Testing Center for None-wood Forest Products of State Forestry Administration (Hangzhou), Fuyang 311400, China
  • Received:2013-09-29 Revised:2013-11-27 Online:2014-02-08 Published:2014-01-25

PDF

224

被引次数

7

摘要：

建立了干食用菌中三价铬(Cr(Ⅲ))和六价铬(Cr(Ⅵ))的液相色谱-电感耦合等离子体质谱(LC-ICP-MS)检测方法。采用微波灰化技术对食用菌样品进行灰化处理，灰化样品用乙二胺四乙酸(EDTA)二钠盐稳定其中的Cr(Ⅲ)，并使其保留在阴离子交换柱(250 mm×4.6 mm，10 μm)上；用含有60 mmol/L硝酸(pH 9.3)的流动相分离其中的Cr(Ⅲ)和Cr(Ⅵ)，电感耦合等离子体质谱仪测定。标准溶液中Cr(Ⅲ)和Cr(Ⅵ)的质量浓度在0.5~50 μg/L范围内呈良好的线性关系，线性回归系数均达到0.9999。食用菌样品中Cr(Ⅲ)和Cr(Ⅵ)不同加入量的平均回收率为78.0%~90.7%，相对标准偏差小于4%(n=6)；定量限均为0.5 μg/L。该方法稳定、可靠、灵敏，可满足干食用菌中Cr(Ⅲ)和Cr(Ⅵ)的测定。

关键词: 干食用菌, 六价铬, 三价铬, 微波灰化, 液相色谱-电感耦合等离子体质谱

Abstract:

An analytical method using liquid chromatography with inductively coupled plasma mass spectrometry (LC-ICP-MS) for the determination of trivalent chromium (Cr(Ⅲ)) and hexavalent chromium (Cr(Ⅵ)) in dried edible fungi was established. Edible fungi sample was ashed by a microwave ashing system and Na2EDTA was added to the ashing sample to stabilize the Cr(Ⅲ). An anion exchange column (250 mm×4.6 mm, 10 μm) with a 60 mmol/L nitric acid (pH 9.3) solution as mobile phase was used for the separation and using ICP-MS as a detector for the determination of trivalent chromium and hexavalent chromium. The calibration curves were linear in the range of 0.5-50 μg/L and the correlation coefficients were 0.9999 for Cr(Ⅲ) and Cr(Ⅵ). The average recoveries of Cr(Ⅲ) and Cr(Ⅵ) ranged from 78.0% to 90.7% with the relative standard deviations (RSDs, n=6) less than 4%. The limits of quantification (LOQ) of Cr(Ⅲ) and Cr(Ⅵ) were 0.5 μg/L. The method is efficient, reliable and sensitive, and can meet the requirement for the determination of Cr(Ⅲ) and Cr(Ⅵ) in dried edible fungi.

Key words: dried edible fungi, hexavalent chromium, liquid chromatography with inductively coupled plasma mass spectrometry (LC-ICP-MS), microwave ashing, trivalent chromium

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