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作 者:曾春城 颜流水[1] 郭会琴[1] 刘宇[1] 杨晓燕[1] 李可心[1]
机构地区:[1]南昌航空大学环境与化学工程学院,南昌330063
出 处:《南昌航空大学学报(自然科学版)》2015年第3期63-69,共7页Journal of Nanchang Hangkong University(Natural Sciences)
基 金:国家自然科学基金资助项目(21165013;21366024);江西省青年科学基金项目(20114BAB213016);江西省重大招标项目(赣科发计字[2010]217号)
摘 要:建立了用毛细管电泳间接紫外检测法分析人发中多种微量金属离子的方法。考察了缓冲液种类,检测波长,缓冲液浓度,缓冲液p H,分离电压及柱温对分离的影响。采用浓度为20 mmol·L-1的咪唑溶液(乙酸调节p H=4.0)作为背景电解液,压力进样(50 mbar×5 s),分离电压15 k V,检测波长214 nm,柱温25℃实验条件下,在7 min内实现了Ca2+、Mg2+、Fe2+、Zn2+、Cu2+5种金属离子的分离与测定。方法的线性范围为0.25~100.00 mg·L-1,检测限为0.10~1.00 mg·L-1,重复5次测定保留时间的相对标准偏差(RSD)小于0.5%,峰面积的相对标准偏差(RSD)小于2.6%。加标回收实验结果较好,回收率为94.3%~104.0%。该方法简单快速,重复性好,准确度高,应用于人发样品的分析,测定结果准确,所测出的金属离子与电感耦合等离子体原子发射光谱法(ICP-AES)测定结果无显著性差异。A method was developed for the determination of trace metal ions in human hair by capillary electrophoresis. The effect factors such as the buffer type,detection wavelength,buffer concentration,buffer p H,separation voltage and column temperature were investigated. Five metal ions of Ca2 +,Mg2 +,Fe2 +,Zn2 +,Cu2 +were separated and determination within 7 min utilizing the concentration of 20 mmol/L imidazole( p H adjusted to 4. 0 by acetic acid) as the background electrolyte solution and the pressure injection( 50 mba × 5 s),the separation voltage of 15 k V,the detection wavelength was set at 214 nm and the column temperature was25 ℃. The linear range ranged from 0. 25 to 100. 00 mg/L,the detection limit ranged from 0. 10 to 1. 00 mg/L. Determination of repeat 5 times,the relative standard deviation( RSD) of retention time was less than 0. 5%,the relative standard deviation( RSD) of peak area was less than 2. 6%. The results of spiked recovery were good and the recoveries were obtained from 94. 3% to 104. 0%.The method was simple,fast,reproducible and high accuracy. The determination resultsofmetal ionswere accurate and had no significant difference compared with inductively coupled plasma atomic emission spectrometry( ICP-AES) when applied to the human hair sample analysis.
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