高效液相色谱-原子荧光光谱法测定慢性砷中毒患者头发中4种形态的砷化合物
Determination of four arsenic species in hair of chronic arsenic poisoning patients by high performance liquid chromatography-atomic fluorescence spectrometry
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摘要:
背景 不同形态的砷化合物毒性差异很大，头发作为慢性砷中毒患者砷的主要蓄积部位，分析其中形态砷的含量对研究人体内砷代谢机制具有重要意义。
目的 建立高效液相色谱-原子荧光光谱（HPLC-AFS）联用技术测定头发中4种形态砷化合物的方法。
方法 实验考察了流动相对色谱分离的影响，通过正交实验优化样品预处理条件和原子荧光（AFS）检测参数，测试了批内、批间、加标回收试验等方法学性能指标。
结果 4种形态的砷化合物即亚砷酸盐（AsⅢ）、砷酸盐（AsⅤ）、一甲基砷酸（MMAⅤ）和二甲基砷酸（DMAⅤ）的线性范围为3.68~100.00 μg/L，相关系数在0.999 1~0.999 6之间，方法检出限为0.11~0.19μg/g，样品加标回收率为96.5%~102.8%，相对标准偏差（RSD）为2.4%~4.3%，浓度为10.00、40.00、80.00μg/L的3个水平样品批内RSD为1.5%~4.4%，批间RSD为1.9%~4.6%。
结论 所建方法具有较高的灵敏度可用于头发中4种形态砷化合物的测定。
Abstract:Background Different arsenic species vary greatly in toxicity. Determinaton of arsenic species in hair has great significance to the study of arsenic metabolism mechanism in human body because hair is the main part to accumulate arsenic in patents with chronic arsenic poisoning.
Objective This study aims to establish a method for determining four arsenic species in hair samples by high performance liquid chromatography-atomic fluorescence spectrometry (HPLC-AFS).
Methods The effect of mobile phase on chromatography separation was investigated. Orthogonal experiment design was used to optimize sample pretreatment conditions and atomic fluorescence spectrometry (AFS) detecton parameters. Methodological indicators were investgated including intra-and inter-batch relatve standard deviatons (RSD) and average spike recovery.
Results The method showed that four arsenic species including arsenite (AsⅢ), arsenate (AsV), monomethylarsonic acid (MMAV), and dimethylarsinic acid (DMAV) were linear within the range of 3.68-100.00 μg/L. The correlaton coefcients were 0.999 1-0.999 6. The limits of detecton were 0.11-0.19 μg/g. The average spike recoveries were 96.5%-102.8% with RSD between 2.4% and 4.3%. The intra-and inter-batch RSDs of repettve measurement at 10.00, 40.00, and 80.00 μg/L were 1.5%-4.4% and 1.9%-4.6% respectvely.
Conclusion The proposed method can be applied to the analysis of four arsenic species in hair samples with high sensitvity.
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