複方甘草合劑錠中所含嗎啡之高效液相層析定量法之研發   全文下載

HPLC Analysis of Morphine in Tablet Mixture Glycyrrhizin Composite

為因應本處產品複方甘草合劑錠品質管理之需，本處曾自行研發經酸鹼處理後以有機溶劑抽提之「抽提法」定量其嗎啡含量；該法樣品量為400錠，約需60個檢驗工時，耗材費時。為改善此缺點，本處乃研發該製劑之嗎啡高效液相層析定量方法。本方法係將檢體以鹼液抽提後經Inertsil 5 ODS-2 管柱（4.6mm × 150mm），以75%含2.5mM sod. 1-dodecanesulfonate之1%醋酸溶液與25% acetonitrile之混合移動相層析之，其他較複雜成分可由提高有機相比例沖提洗出。經取10批本處產品複方甘草合劑錠，依配對試驗（Paired Test）方式分別以抽提法及HPLC法定量其嗎啡。其結果之平均值經平均值推定無顯著差異；標準偏差分別為±1.98%及±1.94%；其相對標準偏差均為0.016。計算10組成對檢驗結果之相關係數得r=0.8093；該相關係數經r-test及t-test均呈非常顯著相關，表示可以HPLC法取代抽提法，而使檢驗樣品量減少至20錠，檢驗工時降低為約8小時，明顯地減低檢驗成本。

For the quality control of morphine content in Tablet Mixture Glycyrrhizin Composite, previously a so called {extraction} method was developed by our bureau. However, this method required acid and base treatments, repeated extraction of the sample with organic solvents, and it took about 60 working-hours. In this study, we have established an HPLC method to determine the morphine content in the product by using an Inertsil 5 ODS-2 colume (4.6 × 150mm), and a mobile phase consisting of 75% 2.5mM sod. 1-dodecane-sulfonate in 1% acetic acid and 25% acetonitrile. In order to compare the HPLC method with extraction method, the morphine content of 1 0 batches of product was quantified by both methods. The results obtained from both methods were not significantly different. The standard deviations of extraction method and HPLC method were ± 1.98% and ± 1.94%, respectively. The correlation coefficient(r) of 10 pairs data was 0.8093, showing very significant relationship between two methods in accordance with the r-and t-tests. In addition, the HPLC method reduces the analysis time to 8 hours. These results strongly suggest that the HPLC method is more efficient than the extraction method.