CAJ | 학술논문

建立了浊点萃取分离原子荧光光谱法测定中药材中痕量汞的方法。Hg2＋可与双硫腙生成疏水性螯合物，水浴加热15 min，鳌合物被萃取到Triton X-114表面活性剂相，经离心与水相分开。在单因素基础上，筛选出对萃取效率有较为显著影响的四因素-溶液pH、Triton X-114浓度、双硫腙浓度和平衡温度，并首次采用Box-Behnken设计和响应面法优化实验参数。结果表明，响应值与因素之间可采用二项式拟合，四个因素的一次项和二次项，以及pH 和Trion X-114、双硫腙交互项对萃取率影响显著，p＜0．05；浊点萃取的最佳条件为：pH 值为5．1，Trion X-114浓度1．16 g·L-1，双硫腙浓度为4．87 mol·L-1，平衡温度为35．6℃，理论荧光值4528．74，实测值与其较接近，仅有2．1％的差别。汞在1～5μg·L-1与荧光值有良好的线性关系，方法检出限为0．01247μg·L-1，RSD为1．30％。该方法成功用于巴戟天、穿心莲和陈皮中汞含量的测定，加标回收率为95．0％～100．0％。Box-Behnken设计结合响应面分析法可以很好的用于浊点萃取条件的优化。
건립료탁점췌취분리원자형광광보법측정중약재중흔량홍적방법。Hg2＋가여쌍류종생성소수성오합물，수욕가열15 min，오합물피췌취도Triton X-114표면활성제상，경리심여수상분개。재단인소기출상，사선출대췌취효솔유교위현저영향적사인소-용액pH、Triton X-114농도、쌍류종농도화평형온도，병수차채용Box-Behnken설계화향응면법우화실험삼수。결과표명，향응치여인소지간가채용이항식의합，사개인소적일차항화이차항，이급pH 화Trion X-114、쌍류종교호항대췌취솔영향현저，p＜0．05；탁점췌취적최가조건위：pH 치위5．1，Trion X-114농도1．16 g·L-1，쌍류종농도위4．87 mol·L-1，평형온도위35．6℃，이론형광치4528．74，실측치여기교접근，부유2．1％적차별。홍재1～5μg·L-1여형광치유량호적선성관계，방법검출한위0．01247μg·L-1，RSD위1．30％。해방법성공용우파극천、천심련화진피중홍함량적측정，가표회수솔위95．0％～100．0％。Box-Behnken설계결합향응면분석법가이흔호적용우탁점췌취조건적우화。
Cloud point extraction (CPE)is proposed as a pre-concentration procedure for the determination of Hg in Chinese herbal medicine samples by hydride generation-atomic fluorescence spectrometry (HG-AFS).Hg2+ was reacted with dithizone to form hydrophobic chelate under the condition of pH.Using Triton X-114,as surfactant,chelate was quantitatively extracted in-to small volume of the surfactant-rich phase by heating the solution in a water bath for 15 min and centrifuging.Four variables including pH,dithizone concentration,Triton X-114 concentration and equilibrium temperature (T)showed the significant effect on extraction efficiency of total Hg evaluated by single-factor experiment,and Box-Behnken design and response surface method-ology were adopted to further investigate the mutual interactions between these variables and to identify their optimal values that would generate maximum extraction efficiency.The results showed that the binomial was used to fit the response to experimental levels of each variable.ALL linear,quadratic terms of four variables,and interactions between pH and Trion X-114,pH and di-thizone affected the response value(extraction efficiency)significantly at 5% level.The optimum extraction conditions were as follows:pH 5. 1,Triton X-114 concentration of 1. 16 g·L-1 ,dithizone concentration of 4. 87 mol·L-1 ,and T 58. 2 ℃,the predicted value of fluorescence was 4 528. 74 under the optimum conditions,and the experimental value had only 2. 1%difference with it.Under the conditions,fluorescence was linear to mercury concentration in the range of 1~5μg·L-1 .The limit of de-tection obtained was 0. 012 47 μg·L-1 with the relative standard deviations (R.S.D.)for six replicate determinations of 1. 30%.The proposed method was successfully applied to determination of Hg in morindae Radix,Andrographitis and dried tan-gerine samples with the recoveries of 95. 0%~100. 0%.Apparently Box- Behnken design combined with response surface anal-ysis method was considered to be well used for optimization of the cloud point extraction.