石墨炉原子吸收法直接测定龙骨水煎液中Cr(Ⅵ)的方法研究  

Study of direct determination of Cr( Ⅵ) in Os. Dracoins decoction by GFAAS

作　　者：王亚丽[1] 金波[1] 马辰[1] 

机构地区：[1]北京协和医学院&中国医学科学院药物研究所,北京100050

出　　处：《药物分析杂志》2014年第5期869-873,共5页Chinese Journal of Pharmaceutical Analysis

基　　金："重大新药创制"科技重大专项(2012ZX09301002-001)

摘　　要：目的：建立石墨炉原子吸收法直接测定六价铬Cr（Ⅵ）的含量。方法：将三氟乙酰丙酮（TFA）和环己烷混匀,再加入pH5.7醋酸-醋酸钠缓冲溶液,三者体积比为1∶2∶2,制得TFA缓冲溶液,采用TFA作为螯合剂与Cr（Ⅲ）在70℃水浴中反应形成可挥发性螯合物CrⅢ（TFA）3,通过石墨炉升温程序使螯合物完全挥发,将Cr（Ⅲ）和Cr（Ⅵ）分离,测定Cr（Ⅵ）的含量。结果：线性范围为0～100 ng·mL-1,回归方程为Y=5.593×10-3X＋7.524×10-3,r=0.9999,样品低、中、高浓度平均回收率分别为98.0%、100.9%、104.5%,精密度试验的RSD为0.58%。结论：本法操作简便,分析速度较快,满足分析测试要求,适于龙骨水煎液中Cr（Ⅵ）含量的测定。Objective： To establish a method for the direct determination of chromium（ Ⅵ） by graphite furnace atomic absorption spectrometry（ GFAAS）. Methods： The trifluoroacetylacetone（ TFA） buffer solution was obtained by mixing TFA with cyclohexane; then the buffer of acetic acid-sodium acetate was added; the volume ratio of these three agents were 1 ∶ 2 ∶ 2. Cr（ Ⅲ） reacted with TFA in water bath at 70 ℃ to form a volatilizable chelate CrⅢ（ TFA）3which was volatilised totally in the GFAAS procedure in order to separate chromium（ Ⅲ） and chromium（ Ⅵ）; then the concentration of chromium（ Ⅵ） was obtained. Results： The linearity of this method ranged from 0 to 100 ng·mL-1; the calibration curve was Y = 5. 593 × 10-3X ＋ 7. 524 × 10-3; the correlation coefficient was 0. 9999; the average spiked recoveries were 98. 0%,100. 9%,104. 5% at low,medium and high concentrations,respectively; RSD of precision test was 0. 58%. Conclusion： This method is accurate,simple,feasible and rapid, which met the analytical requirement and could be used for the determination of chromium（ Ⅵ） in Os. Dracoins decoction.

关 键 词：六价铬 石墨炉原子吸收法 三氟乙酰丙酮 挥发性螯合物 龙骨水煎液 

分 类 号：R917[医药卫生—药物分析学]