液相色谱-原子荧光光谱法测定大米中无机砷形态
|
摘要
建立了液相色谱-原子荧光法测定大米中无机砷形态的检测方法,对流动相种类、流速、pH值、硼氢化钾浓度及盐酸浓度进行了优化。在8 min内可完成As(Ⅲ)和As(Ⅴ)的分离。当砷酸根和亚砷酸根浓度为0~100ng/ml时,2种形态均可得到良好的线性关系,线性相关系数均大于等于0.999 5,实验室检出限分别为0.006mg/kg和0.009mg/kg,精密度RSD≤6.0%,加标回收率为85.0%~110.7%。该方法减少了样品的分析时间和试剂用量,具有简便、高效和可靠等特点,可用于大米中无机砷形态的检测。
The method was established to determine inorganic arsenic species in rice by liquid chromatography-atomic fluorescence spectrometry.Types of mobile phase,flow rate,pH,the concentrations of potassium borohydride and hydrochloric acid were optimized.Arsenous acid radical and arsenic acid radical can be separated in 8min.Arsenous acid radical and arsenic acid radical had good linear relationships with the concentrations of the forms ranging from 0to 100ng/ml,and the linear correlation coefficients of standard was more than 0.999 5,the laboratory detection limits of arsenous acid radical and arsenic acid radical were 0.006mg/kg and 0.009mg/kg,the RSDof the precision of method was less than 6.0%.And the recovery rate of standard addition applied to the sample was 85.0%~110.7%.Inorganic arsenic species detection by LC-AFS was a simple,efficient and reliable method with less analysis time and reagent dosage,and was feasible for analysis of inorganic arsenic species in rice.
The method was established to determine inorganic arsenic species in rice by liquid chromatography-atomic fluorescence spectrometry.Types of mobile phase,flow rate,pH,the concentrations of potassium borohydride and hydrochloric acid were optimized.Arsenous acid radical and arsenic acid radical can be separated in 8min.Arsenous acid radical and arsenic acid radical had good linear relationships with the concentrations of the forms ranging from 0to 100ng/ml,and the linear correlation coefficients of standard was more than 0.999 5,the laboratory detection limits of arsenous acid radical and arsenic acid radical were 0.006mg/kg and 0.009mg/kg,the RSDof the precision of method was less than 6.0%.And the recovery rate of standard addition applied to the sample was 85.0%~110.7%.Inorganic arsenic species detection by LC-AFS was a simple,efficient and reliable method with less analysis time and reagent dosage,and was feasible for analysis of inorganic arsenic species in rice.
引文
[1]姚晶晶,袁友明,王明锐,等.高效液相色谱-氢化物发生-原子荧光法测定大米中的4种砷形态[J].光谱仪器与分析,2012(4):37-39.
[2]MANDAL B K,SUZUKI K T.Arsenic round the world:A review[J].Talanta,2002,58:201-235.
[3]净锦飞,徐焰,骆文静,等.亚慢性砷暴露对大鼠肾脏功能和形态的影响[J].实用预防医学,2011,18(2):195-198.
[4]LE X C,LU X F,LI X F.Arsenic speciation[J].Anal chen,2004,76(1):27.
[5]倪张林,屈明华,丁明.原子荧光光谱法测定海藻肥中的总砷和无机砷[J].光谱实验室,2010,27(2):573-576.
[6]潘仁凯,江映.原子荧光光谱法测定土壤中的As(Ⅲ)和As(Ⅴ)[J].内蒙古石油化工,2010(1):14-15.
[7]张华,王英锋,施燕支,等.高效液相色谱及联用技术在砷形态分析中的应用[J].光谱学与光谱分析,2007,27(2):386-390.
[8]刘锋,石志芳,姜霞,等.HPLC-ICP-MS法分析太湖沉积物中砷的形态及分布特征[J].质谱学报,2011,32(3):170-175.
[9]安艳,李贞,王三祥,等.HPLC-ICP-MS在砷形态分析中应用[J].中国公共卫生,2008,24(2):1 416-1 418.
[10]TOWNSEND A T,SULLIVANJO,FEATHERSTONE A M,et al.Sampling and analysis for arsenic dissolved in ground water and surface water[J].J Environ Monit,2001,21(3):113-120.
[11]薛慧,董宾,宫博,等.方便面中砷元素的形态分析[J].化学分析计量,2013(6):49-52.
[2]MANDAL B K,SUZUKI K T.Arsenic round the world:A review[J].Talanta,2002,58:201-235.
[3]净锦飞,徐焰,骆文静,等.亚慢性砷暴露对大鼠肾脏功能和形态的影响[J].实用预防医学,2011,18(2):195-198.
[4]LE X C,LU X F,LI X F.Arsenic speciation[J].Anal chen,2004,76(1):27.
[5]倪张林,屈明华,丁明.原子荧光光谱法测定海藻肥中的总砷和无机砷[J].光谱实验室,2010,27(2):573-576.
[6]潘仁凯,江映.原子荧光光谱法测定土壤中的As(Ⅲ)和As(Ⅴ)[J].内蒙古石油化工,2010(1):14-15.
[7]张华,王英锋,施燕支,等.高效液相色谱及联用技术在砷形态分析中的应用[J].光谱学与光谱分析,2007,27(2):386-390.
[8]刘锋,石志芳,姜霞,等.HPLC-ICP-MS法分析太湖沉积物中砷的形态及分布特征[J].质谱学报,2011,32(3):170-175.
[9]安艳,李贞,王三祥,等.HPLC-ICP-MS在砷形态分析中应用[J].中国公共卫生,2008,24(2):1 416-1 418.
[10]TOWNSEND A T,SULLIVANJO,FEATHERSTONE A M,et al.Sampling and analysis for arsenic dissolved in ground water and surface water[J].J Environ Monit,2001,21(3):113-120.
[11]薛慧,董宾,宫博,等.方便面中砷元素的形态分析[J].化学分析计量,2013(6):49-52.