详细信息
短柱分离-电感耦合等离子体质谱联用测定大米和紫菜中的无机砷 被引量:4
Determination of inorganic arsenic species in rice and laver by liquid chromatography-inductively coupled plsama mass spectrometry with C_8 reversed-phase chromatogram column
文献类型:期刊文献
中文题名:短柱分离-电感耦合等离子体质谱联用测定大米和紫菜中的无机砷
英文题名:Determination of inorganic arsenic species in rice and laver by liquid chromatography-inductively coupled plsama mass spectrometry with C_8 reversed-phase chromatogram column
作者:倪张林[1,2] 汤富彬[1,2] 喻晴[1,2] 莫润宏[1,2]
第一作者:倪张林
机构:[1]中国林业科学研究院亚热带林业研究所;[2]国家林业局经济林产品质量检验检测中心(杭州)
年份:2014
卷号:33
期号:12
起止页码:1392-1396
中文期刊名:分析试验室
外文期刊名:Chinese Journal of Analysis Laboratory
收录:CSTPCD;;北大核心:【北大核心2011】;CSCD:【CSCD2013_2014】;
基金:中央级公益性科研院所基本科研业务费专项资金(RISF2013011);国家林业公益性行业科研专项(201204414)资助
语种:中文
中文关键词:液相色谱-电感耦含等离子体质谱;大米;紫菜;无机砷
外文关键词:LC-ICP-MS; Rice; Laver; Inorganic arsenic
分类号:O657.63
摘要:建立了C8反相色谱短柱分离-电感耦合等离子体质谱联用技术(LCICP-M S)测定大米和紫菜中无机砷的检测方法。样品用含有2%H2O2的流动相在1000W大功率超声进行萃取(70℃,50 min),使其中的无机砷转化为五价砷,以1 mmol/L KH2PO4+1 mmol/L四丁基氢氧化铵(p H 5.5)为流动相,经C8反相色谱柱分离,电感耦合等离子体质谱仪进行定量分析。方法学验证表明:在0.5-50μg/L范围内无机砷线性良好,线性相关系数(r2)为0.9996,定量限(LOQ)为0.3μg/L,加标回收率在85.2%-109%之间,相对标准偏差(RSD,n=6)在2.1%-4.4%。方法适合于批量测定大米和紫菜样品中的无机砷。
A method for the analysis of inorganic arsenic in rice and laver by liquid chromatography- inductively coupled plasma mass spectrometry( LC- ICP- MS) has been proposed. Rice and laver were extracted by ultrasonic with the power of 1000W( 70℃,50min). 1mmol / L potassium dihydrogen phosphate + 1mmol / L tetrabutyl ammonium hydroxide( TBAOH) with 3% hydrogen peroxide( V / V) was used as extraction solvent that could convert all forms of inorganic arsenic to pentavalent arsenic in extraction process. The LC separation was performed on a C8reversed- phase chromatographic column utilizing a isocratic elution program with1 mmol / L potassium dihydrogen phosphate( p H 5. 5) as the mobile phase. Methodology validation showed that linear correlation coefficient( r) for inorganic arsenic was 0. 9996 at 0. 5 - 50 μg / L and quantitative limit( LOQ) was 0. 3 μg /L. The recoveries were between 85. 2% and 109% with relative standard deviations( RSD,n = 6) of 2. 1% - 4. 4%. The method was efficient,reliable and sensitive,which could meet requirement for the determination of inorganic arsenic in rice and laver.
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