透過重氮化反應檢測藥劑及尿液中 Metoclopramide 含量   全文下載

Determination of Metoclopramide Hydrochloride in Pharmaceuticals and Spiked Human Urine through Diazotization Reaction

本研究敘述三種簡單，快速，靈敏和具成本效益的滴定法和分光光度法測定Metoclopramide（MCP）藥劑及尿液中含量。滴定法是基於重氮化反應涉及MCP的一級胺群組在酸性介質中和亞硝酸鈉反應的視覺（方法A）和電位（方法B）終點測定。分光光度法（方法C）取決於重氮化的MCP與二苯胺偶合，產生最大吸收波長530 nm的紅色光。實驗條件已最佳化。兩種滴定方法適用濃度範圍在1.0 - 20.0 mg，且MCP：亞硝酸鈉為1：1時的化學計量反應計算。分光光度法在濃度範圍0.3 - 7.5 μg/mL時符合比爾定律，摩爾吸光係數為4.73×104 L/mol cm，桑德爾靈敏度為0.007 μg/cm2。檢測極限和定量極限分別為0.22和0.67 μg/mL。本研究方法適用於MCP錠劑、注射劑和尿液的檢測。

Three simple , rapid, sensitive and cost-effective titrimetric and spectrophotometric methods were described for the determination of metoclopramide (MCP) in its pharmaceutical dosage forms and spiked human urine. The titrimetric methods were based on the diazotiza-tion reaction involving the primary amine group of MCP and NaNO2 in acid medium with visual (method A) and potentiometric (method B) end point detection. The spectrophotometric method (method C) depends upon the diazotization of MCP in acid medium followed by coupling with diphenylamine to give a red colored chromogen with a wavelength of maximum absorption at 530 nm. The experimental conditions were optimized. Both the titrimetric methods were applicable over the concentration range of 1.0 - 20.0 mg and the calculations were based on a 1 : 1 (MCP: NaNO2) reaction stoichiometry. In the spectrophotometric method, Beer’s law was obeyed over the concentra-tion range of 0.3 - 7.5 µg/mL with a molar absorptivity of 4.73 × 104 L/mol cm and Sandell’s sensitivity being 0.007 μg/cm2. The limit of detection and the limit of quantification were calculated to be 0.22 and 0.67 µg/mL, respectively. The proposed methods were applied to the determination of MCP in tablets, injection and also in spiked human urine.