食品科学 ›› 2022, Vol. 43 ›› Issue (6): 331-336.doi: 10.7506/spkx1002-6630-20210503-013

• 安全检测 • 上一篇    下一篇

氢化物发生-电感耦合等离子体串联质谱法分析大米中的无机砷

李爱阳,黄建华   

  1. (1.湖南工学院材料科学与工程学院,湖南衡阳 421002;2.湖南中医药研究院中医研究所,湖南长沙 410013)
  • 出版日期:2022-03-25 发布日期:2022-03-28
  • 基金资助:
    国家自然科学基金青年科学基金项目(81603400);湖南省自然科学基金项目(2019JJ60026); 湖南省教育厅重点项目(20A140);湖南省应用特色学科材料科学与工程学科项目(湘教通[2018]469号); 湖南省工程研究中心项目(湘发改委高技[2019]853号)

Inorganic Arsenic Analysis in Rice by Hydride Generation Inductively Coupled Plasma-Tandem Mass Spectrometry

LI Aiyang, HUANG Jianhua   

  1. (1. School of Material Science and Engineering, Hunan Institute of Technology, Hengyang 421002, China; 2. Institute of Chinese Materia Medica, Hunan Academy of Traditional Chinese Medicine, Changsha 410013, China)
  • Online:2022-03-25 Published:2022-03-28

摘要: 建立氢化物发生-电感耦合等离子体串联质谱(inductively coupled plasma-tandem mass spectrometry,ICP-MS/MS)法直接测定大米中无机砷含量的高通量分析方法。采用硝酸-双氧水提取大米样品中的无机砷,以5 mol/L盐酸作为预还原剂将砷(V)还原为砷(III),在多模式样品导入系统中利用2 g/100 mL硼氢化钠溶液将无机砷(III)还原为挥发性胂(AsH3),导入ICP-MS/MS直接进行测定;在MS/MS模式下,采用氧气为反应气,将砷转移为氧化砷消除质谱干扰,砷的检出限为0.004 μg/L。方法用于分析标准参考物质大米粉(GBW(E)100348a、GBW(E)100349a、NIST SRM1568b)中无机砷,测定结果与参考物质的认定值基本一致,验证方法准确性好。方法无需与色谱技术联用进行砷的形态分离也能单独测定大米中的无机砷,具有操作简单快速、灵敏度高、准确可靠的特点,适用于大米中无机砷含量的测定。

关键词: 大米;无机砷;电感耦合等离子体串联质谱;氢化物发生;多模式样品导入系统

Abstract: A high throughput analytical method for the direct determination of inorganic arsenic content in rice by hydride generation (HG) inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS) was established. Inorganic arsenic was extracted from rice samples with a mixture of nitric acid and hydrogen peroxide. Arsenic (V) was pre-reduced into arsenic (III) by adding 5 mol/L hydrochloric acid, and then 2 g/100 mL sodium borohydride solution was used to reduce inorganic arsenic (III) into volatile arsenic hydride (AsH3) in a multimode sample introduction system (MSIS). Finally, AsH3 was injected into the ICP-MS/MS system and directly detected. In the MS/MS mode, arsenic was transferred to arsenic oxide using oxygen as reaction gas to eliminate the mass spectral interference. The limit of detection (LOD) for arsenic was 0.004 μg/L. The results of the method for inorganic arsenic in standard reference materials of rice flour (GBW(E)100348a, GBW(E)100349a, and NIST SRM1568b) were consistent with the certified values, indicating good accuracy of the method. Inorganic arsenic in rice could be detected using this method without chromatographic separation of different arsenic species. This method was characterized by simple and rapid operation, high sensitivity, good accuracy and high reliability, and applicable for the determination of inorganic arsenic content in rice.

Key words: rice; inorganic arsenic; inductively coupled plasma-tandem mass spectrometry; hydride generation; multimode sample introduction system

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