Andac Muberra, Asan Adem, Bekdemir Yunus, Kutuk Halil, Isildak Ibrahim
Department of Chemistry, Faculty of Science, Ondokuz Mayis University, 55139 Kurupelit-Samsun, Turkey.
Talanta. 2003 May 28;60(1):191-7. doi: 10.1016/S0039-9140(03)00122-X.
A new, simple and rapid spectrophotometric FI method for the accurate and precise determination of Hg(II) in pharmaceutical preparations has been developed. The method is based on the measuring the decrease of absorbance intensity of p-nitrobenzoxosulfamate (NBS) due to the complexation with Hg(II). The absorption peak of the NBS, which is decreased linearly by addition of Hg(II), occurs at 430 nm in 2x10(-4) moll(-1) HNO(3) as a carrier solution. Optimization of chemical and FI variables has been made. A micro column consisting of several packing materials applied instead of reaction coil was also investigated. A background level of Fe(III) maintained in reagent carrier solution with NBS was found useful for sensitivity and selectivity. Under the optimized conditions, the sampling rate was over 100 h(-1), the calibration curve obtained were linear over the range 1-10 mugml(-1), the detection limit was lower than 0.2 mugml(-1) for a 20 mul injection volume, and the precision [S(r)=1% at 2 mugml(-1) Hg(II) (n=10)] was found quite satisfactory. Application of the method to the analysis of Hg(II) in pharmaceutical preparations resulted a good agreement between the expected and found values.
已开发出一种用于准确、精确测定药物制剂中汞（II）的新型、简单且快速的分光光度流动注射法。该方法基于测量对硝基苯并氧代磺酸酯（NBS）因与汞（II）络合而导致的吸光度强度降低。NBS的吸收峰在2×10⁻⁴mol·L⁻¹HNO₃作为载液时于430nm处出现，加入汞（II）后该吸收峰呈线性下降。已对化学和流动注射变量进行了优化。还研究了用几种填充材料组成的微柱代替反应盘管的情况。发现用NBS在试剂载液中保持一定水平的铁（III）背景对灵敏度和选择性很有用。在优化条件下，进样速率超过100h⁻¹，得到的校准曲线在1 - 10μg·ml⁻¹范围内呈线性，对于20μl进样体积，检测限低于0.2μg·ml⁻¹，精密度[在2μg·ml⁻¹汞（II）时S（r） = 1%（n = 10）]相当令人满意。将该方法应用于药物制剂中汞（II）的分析，预期值与实测值之间具有良好的一致性。
