Liu Yi-Xiang, Wu Yong-Pei, Wang Li, Huang Zhi-Yong
Bioengineering School of Jimei University, Xiamen 361021, China.
Guang Pu Xue Yu Guang Pu Fen Xi. 2008 Nov;28(11):2691-4.
In the present article, the method of high pressure microwave digestion and hydride generation atomic fluorescence spectroscopy (HG-AFS) was used for the determination of total arsenic and mercury in fucoidans, and the detecting conditions were optimized, including instrument working parameters, such as atomic temperature, lamp current, high voltage of PMT etc, and the conditions of hydride generation, such as the acid concentration of loading fluid, speed of carrying gas, the concentration of KBH4 etc. The result shows that there are good linear relations between fluorescence intensity and the concentrations of arsenic and mercury where their concentrations are 0-200 microg x L(-1) and 2.0-10.0 microg x L(-1), respectively, and the related coefficient of arsenic is 0. 999 9 and that of mercury's is 0. 999 8. The blanks of samples were detected constantly (n = 10), and the detection limit of this method is 0.173 ng x kg(-1) for total arsenic and 0.012 2 ng x kg(-1) for mercury. In order to do precise analysis, the samples were detected constantly (n = 8), and the relative standard deviations (RSDs) of arsenic and mercury are 1.09% and 1.69%, severally. The quantitative arsenic and mercury were added into the samples before they were digested, and the recovery range is 93.31%-100.9% for arsenic and 91.21%-106.1% for mercury. The contents of total arsenic and mercury in fucoidans before desalted by ultrafiltration are 2.78 mg and 0.125 mg x kg(-1), respectively. Nevertheless, the contents of total arsenic and mercury in fucoidans desalted by ultrafiltration are 2.26 mg x kg(-1) and 0.119 mg x kg(-1), severally.
本文采用高压微波消解 - 氢化物发生原子荧光光谱法(HG - AFS)测定岩藻聚糖中的总砷和汞,并对检测条件进行了优化,包括仪器工作参数,如原子化温度、灯电流、光电倍增管高压等,以及氢化物发生条件,如载流酸浓度、载气流量、硼氢化钾浓度等。结果表明,荧光强度与砷和汞浓度在0 - 200 μg·L⁻¹和2.0 - 10.0 μg·L⁻¹范围内分别呈良好线性关系,砷的相关系数为0.999 9,汞的相关系数为0.999 8。对样品空白进行连续测定(n = 10),该方法对总砷的检出限为0.173 ng·kg⁻¹,对汞的检出限为0.012 2 ng·kg⁻¹。为进行精确分析,对样品进行连续测定(n = 8),砷和汞的相对标准偏差(RSD)分别为1.09%和1.69%。在样品消解前加入定量的砷和汞,砷的回收率范围为93.31% - 100.9%,汞的回收率范围为91.21% - 106.1%。超滤脱盐前岩藻聚糖中总砷和汞的含量分别为2.78 mg·kg⁻¹和0.125 mg·kg⁻¹。然而,超滤脱盐后岩藻聚糖中总砷和汞的含量分别为2.26 mg·kg⁻¹和0.119 mg·kg⁻¹。