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微波辅助萃取-离子色谱-动态反应池电感耦合等离子体质谱法用于谷物中砷和硒的形态分析

Microwave-assisted extraction and ion chromatography dynamic reaction cell inductively coupled plasma mass spectrometry for the speciation analysis of arsenic and selenium in cereals.

作者信息

Tsai Chia-Ying, Jiang Shiuh-Jen

机构信息

Department of Chemistry, National Sun Yat-sen University, Kaohsiung, Taiwan.

出版信息

Anal Sci. 2011;27(3):271-6. doi: 10.2116/analsci.27.271.

Abstract

An ion chromatography dynamic reaction cell inductively coupled plasma mass spectrometric (IC-DRC-ICP-MS) method for the speciation of arsenic and selenium compounds is described. Chromatographic separation was performed in a gradient elution mode using 0.5 mmol L(-1) ammonium citrate in 1% methanol (pH 4.5) and 15 mmol L(-1) ammonium citrate in 1% methanol (pH 8.0). The potentially interfering (38)Ar(40)Ar(+) and (40)Ar(40)Ar(+) at selenium masses of m/z 78 and 80 were reduced in intensity by approximately 3 orders of magnitude by using 1.0 mL min(-1) CH(4) as a reactive cell gas in the DRC. Arsenic was determined as the adduct ion (75)As(12)CH(2)(+) at m/z 89. The detection limits of the procedure were in the ranges of 0.006-0.009 ng As mL(-1) and 0.009-0.03 ng Se mL(-1), respectively. This method has been applied to determine various arsenic and selenium compounds in cereal samples. The accuracy of the method has been verified by comparing the sum of the concentrations of individual species obtained by the present procedure with the total concentration of elements. The arsenic and selenium compounds were quantitatively extracted with a Protease XIV and α-amylase solution in a microwave field at 70°C during a period of 30 min. The spike recoveries were in the range of 94-105% for all determinations.

摘要

描述了一种用于砷和硒化合物形态分析的离子色谱动态反应池电感耦合等离子体质谱法(IC-DRC-ICP-MS)。采用梯度洗脱模式进行色谱分离,流动相为含1%甲醇的0.5 mmol L⁻¹柠檬酸铵(pH 4.5)和含1%甲醇的15 mmol L⁻¹柠檬酸铵(pH 8.0)。通过在动态反应池中使用1.0 mL min⁻¹ CH₄作为反应气,m/z 78和80处硒质量数下潜在干扰的³⁸Ar⁴⁰Ar⁺和⁴⁰Ar⁴⁰Ar⁺强度降低了约3个数量级。砷以m/z 89处的加合离子⁷⁵As¹²CH₂⁺形式测定。该方法的检测限分别在0.006 - 0.009 ng As mL⁻¹和0.009 - 0.03 ng Se mL⁻¹范围内。此方法已应用于测定谷物样品中的各种砷和硒化合物。通过将本方法得到的各形态浓度之和与元素总浓度进行比较,验证了该方法的准确性。在70°C的微波场中,用蛋白酶XIV和α -淀粉酶溶液在3分钟内对砷和硒化合物进行定量提取。所有测定的加标回收率在94% - 105%范围内。

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