炭黑氨基柱净化-HPLC-ICP-MS测定黄酒中铬价态及含量

建立了一种测定黄酒中Cr（Ⅲ）、Cr（Ⅵ）的高效液相色谱-电感耦合等离子体质谱分析方法。黄酒经炭黑氨基柱净化,超纯水洗脱,色谱条件为:Dionex AS11-HC阴离子预柱（4 mm×50 mm×9μm）;以60 mmol/L（p H9.0）硝酸铵作为流动相,流量为1.5 m L/min;以电感耦合等离子体质谱进行定性和定量分析。结果表明:在0²0μg/L范围内Cr（Ⅲ）、Cr（Ⅵ）线性良好,相关系数R2均在0.998以上;添加回收率在81.2%⁹4.8%之间,相对标准偏差为1.7%⁴.1%;定量限分别为0.12μg/L和0.18μg/L。本方法简单快速,适用于黄酒中铬形态残留的分析检测,并利用该方法对不同年份、不同企业及不同类型的黄酒进行了检测,发现绍兴地区的黄酒中的铬主要以Cr（Ⅲ）形态存在。 

Determination of chromium species and content in rice wine by high performance liquid chromatography- inductively coupled plasma mass spectrometry

A high performance liquid chromatography and inductively coupled plasma mass spectrometry ( HPLCICP- MS) method was developed for determination of Cr ( Ⅲ) , Cr ( Ⅵ) in rice wine. The wine sample was purified with Carb- NH2 SPE column, eluted with ultra- pure water and then separated on a Dionex AS11- HC ( 4 mm × 50 mm × 9 μm) column using 60 mmol / L ammonium nitrate ( p H9.0) at 1.5m L / min as mobile phase. Identification and quantification were achieved by inductively coupled plasma mass spectrometry ( ICP- MS) . It showed good liner correlation between 0 and 20 μg / L with correlation coeficients better than 0.998.The average recoveries of Cr ( Ⅲ) and Cr ( Ⅵ) ranged from 81.2% to 94.8% at different spiked level sand the relative standard deviations ranged from1.7% to 4.1%.The quantification limits of Cr ( Ⅲ) and Cr ( Ⅵ) were 0.12 μg / L and 0.18 μg / L respectively.The method was suited for determination of chromium species in rice wine.Shao xing rice wines of different kind and different age from different manufacturers were determinted using the established method, results showed that Cr ( Ⅲ) was the main specie.