頭袍子菌素類抗素雪華若林酸鹽轉化與醇－水系統溶解度之研究

雪華若林屬於丙－內醯氨（β-lactam）類抗生素，有良好的抗菌性，尤其是對大腸桿菌的抑制特別有效。本實驗以商品雪華若林鈉鹽（簡稱CEZ-COONa）為起始原料，模擬工業製程，先製成雪華若林酸（簡稱CEZ-COOH），然後再製成鈉鹽結晶。求其酸化條件及回收率與酸鹽轉化過程之最佳鹽化劑及最後再結晶產物之純度。並比較產物與原料之紅外線吸收光譜，確認產物晶型及含結晶水之特性。雪華若林鈉鹽在15°Ｃ、25°Ｃ、40°Ｃ時由甲醇-水，乙醇-水之溶劑系統所得之溶解庋曲線圖顯示，在雪華若林鈉鹽-乙醇-水系統中，溫度愈高，溶解度愈高；而在雪華若林鈉鹽-甲醇-水系統中，當甲醇含量較少時，以在25°Ｃ時之溶解度最高，40°Ｃ次之，而以在15°Ｃ時最少 ; 當甲醇含量增加時，在15°Ｃ時之溶解度有愈來愈高而在40°Ｃ時之溶解度有成為最少之趨勢。商品雪華若林鈉鹽經過20%甲醇水溶液，以6N鹽酸控制pH為1.23，在25°Ｃ下經攪拌一小時後，得雪華若林酸白色粉末，經過濾乾燥，其回收率達90%。以此雪華若林酸在二乙基己烷鈉鹽及乙醇溶液中進行雪華若林鈉鹽製備可得超過90%的回收率且純度可達95%。再製得之結晶與商品雪華若林鈉鹽之紅外線吸收光譜此較顯示相近的特性。

關鍵字

雪華若林；丙-內醯氨；抗生素；溶解度；高效液相層析；紅外線光譜

並列摘要

Cefazolin belongs to β-lactam antibiotics, having a broad spectrum of antibacterial activity especially for Escherichia coli. In this study commercial cefazolin sodium (CEZ-COONa) was used as starting material to simulate the industrial separation and purification processes. The first step was to make cefazolin free acid (CEZ-COOH), and then to make cefazolin sodium crystalline. We obtained cefazolin sodium solubility diagrams of the solvent system methanol-water, ethanol-water at 15℃, 25℃, and 40℃, respectively. The higher the temperature, the higher the solubility in the cefazolin sodium-ethanol-water system. But the higher the temperature, the less the solubility when the amount of methanol was gradually increased in the cefazolin sodium-methanol-water system. Cefazolin sodium dissolved in 20% methanol solution was further adjusted to pH 1.23 at 25℃ and then agitated for 1 hour; then, we obtained a white cefazolin free acid powder, the recovery was about 90%. Taking the cefazolin free acid into a solution of sodium 2-ethyl hexanoate and ethanol, a crystalline salt cefazolin sodium was produced. The recovery was about 90% and the purity was about 95% analyzed by HPLC. The characteristics of the recrystallized product was similar to the cefazolin sodium starting material standard in the IR spectrum.

並列關鍵字

cefazolin ； β-lactam ； antibiotic ； Solubility ； HPLC ； IR

國際替代計量

頭袍子菌素類抗素雪華若林酸鹽轉化與醇－水系統溶解度之研究

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