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題名 | Comparative Study of Electrospray Mass Spectrometry and First Derivative Method and Validation by HPLC Method=電噴霧離子源質譜法、一次微分法及HPLC法確效之比較研究 |
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作者 | Özdemir, Abdil; Korkmaz, Ayşenur; |
期刊 | 藥物食品分析 |
出版日期 | 20070600 |
卷期 | 15:2 2007.06[民96.06] |
頁次 | 頁118-125+207 |
分類號 | 418.43 |
語文 | eng |
關鍵詞 | 一次微分; 電噴霧離子源質譜; Klavulanate-鉀; Amoxicillin; Potassium Klavulanate; First derivative; Electrospray mass spectrometry; HPLC; |
中文摘要 | 本文介紹了三種方法,以同時測定合成藥物中amoxicillin trihydrate(AMX)和potassium klavulanate(KLV)。第一種方法使用紫外光譜一次微分和零點穿越測量。第二種方法是基於電噴霧離子源質譜。在電噴霧的研究中,阿斯匹靈 (ASP)及克林達黴素(CLN)被分別做爲正離子和負離子的定量測量之內標準品。校正曲線是建立在與一次微分方法相同的範圍內。反相高效液相層析 (RP-HPLC)和紫外光檢測(λ=220nm)的方法被使用來分析AMX和KLV。層析採用C18管柱,以含磷酸鹽的乙腈(40:60,v/v)爲流動相,流速0.8ml/min。方法的選擇性、檢測極限、回收率、準確性和精確度在實驗中被驗證。對於兩種藥物,AMX在21-49μg/ml和KLV 3-7μg/mL範圍內,在本方法具有良好的選擇性、線性(R≈0.99)、準確性(回收率=100-105%)和精確性(<3% RSD)。三種方法的最低的檢測極限和最低定量極限都被測定。 |
英文摘要 | Three different methods are described for the simultaneous determination of amoxicillin trihydrate (AMX) and potassium klavulanate (KLV) in synthetic mixtures and pharmaceutical tablets. The first method depends on the first-derivative ultraviolet spectrophotometry with zero-crossing measurement. The second method is based on mass spectrometry utilizing electropspray ionization. For the electrospray studies in negative and positive ion modes, aspirin (ASP) and clindamycin (CLN) were used, respectively as internal standards for quantification. The calibration function was established in the same concentration ranges as in the first derivative method. A reversed-phase high performance liquid chromatographic (RP-HPLC) method involving ultraviolet detection (λ= 220 nm) was developed for the analysis of AMX and KLV. Chromatography was carried out on a C-18 column with mobile phase comprising of phosphate buffer-acetonitrile (40:60, v/v). The proposed methods have been validated with regard to the selectivity, detection limit, recovery, accuracy and precision. For both drugs, methods were found to be selective, linear (R ≈ 0.99), accurate (recovery = 100-105%) and precise (<3% RSD) in the range of 21-49 µg/mL for AMX and 3-7 µg/mL for KLV. The limit-of-detection and limit-of-quantification of the method were determined for three methods. |
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