Ahmed Manzoor, Asghar Muhammad, Yaqoob Mohammad, Munawar Nusrat, Shahid Farkhanda, Asad Mida, Nabi Abdul
Department of Chemistry, University of Balochistan.
Department of Chemistry, Sardar Bahadur Khan Women University.
Anal Sci. 2017;33(11):1259-1263. doi: 10.2116/analsci.33.1259.
Diperiodatoargentate(III) (DPA)/silver(III) complex, [Ag(HIO)], in sulfuric acid medium has been used to determine hyoscine butylbromide (HBB) by flow injection (FI) coupled with chemiluminescence (CL) detector. A linear standard curve between the CL intensity and concentration range from 0.005 to 20 mg L was obtained. The determination coefficient (R), limit of detection (3s × blank), relative standard deviation (RSD) for 0.5 mg L HBB and analytical throughput were 0.9992 (n = 8), 5 × 10 mg L, 1.5% (n = 10) and 160 injections h, respectively. The developed method was applied for the determination of HBB in pharmaceutical formulations with recoveries from 92 ± 4 to 108 ± 3%. For comparison, a spectrophotometric method was used and the results obtained by both methods were in good agreement at a 95% confidence level. The effect of key chemical and physical variables (reagent concentration, flow rate, sample volume, PMT voltage) and interfering species (pharmaceutical excipients and inorganic ions) on the determination of HBB was examined. The possible CL mechanism of HBB on silver(III) complex in sulfuric acid medium was also discussed in brief.
在硫酸介质中，二过碘酸根合银（III）（DPA）/银（III）配合物[Ag(HIO)]已被用于通过流动注射（FI）结合化学发光（CL）检测器来测定丁溴东莨菪碱（HBB）。获得了化学发光强度与浓度在0.005至20 mg/L范围内的线性标准曲线。对于0.5 mg/L的HBB，测定系数（R）、检测限（3s×空白）、相对标准偏差（RSD）（n = 10）和分析通量分别为0.9992（n = 8）、5×10 mg/L、1.5%和160次进样/小时。所建立的方法用于药物制剂中HBB的测定，回收率为92±4%至108±3%。为作比较，采用了分光光度法，两种方法在95%置信水平下所得结果吻合良好。考察了关键化学和物理变量（试剂浓度、流速、样品体积、光电倍增管电压）和干扰物质（药物赋形剂和无机离子）对HBB测定的影响。还简要讨论了HBB在硫酸介质中与银（III）配合物反应可能的化学发光机理。
