加校正因子的RP-HPLC法測(cè)定不同方法生產(chǎn)的7-氨基頭孢烷酸中有關(guān)物質(zhì)
發(fā)布時(shí)間:2018-04-25 18:00
本文選題:高效液相色譜法 + -氨基頭孢烷酸; 參考:《中國(guó)抗生素雜志》2015年01期
【摘要】:目的建立一種能夠準(zhǔn)確測(cè)定7-氨基頭孢烷酸中有關(guān)物質(zhì)的方法,同時(shí)進(jìn)行不同方法生產(chǎn)的產(chǎn)品的含量測(cè)定及有關(guān)物質(zhì)檢查。方法采用高效液相色譜法。使用C18色譜柱(SB-C18,5μm,4.6mm×250mm);以磷酸鹽緩沖液(取5g磷酸氫二鉀和5g磷酸二氫鉀溶解于1000m L水中,用磷酸調(diào)節(jié)流動(dòng)相p H值至6.0)—乙腈(92:8)為流動(dòng)相;檢測(cè)波長(zhǎng)為254nm;柱溫為35℃;進(jìn)樣量20μL。結(jié)果 7-氨基頭孢烷酸在504~0.02534μg/m L范圍內(nèi),線性關(guān)系良好,相關(guān)系數(shù)R2為0.9991;去乙酰7-氨基頭孢烷酸在10.52~0.0263μg/m L范圍內(nèi),線性關(guān)系良好,相關(guān)系數(shù)R2為0.9996;去乙酰氧7-氨基頭孢烷酸在9.66~0.02415μg/m L范圍內(nèi),線性關(guān)系良好,相關(guān)系數(shù)R2為0.9998;頭孢菌素C在10.5~0.02625μg/m L范圍內(nèi),線性關(guān)系良好,相關(guān)系數(shù)R2為0.9998。溶液的穩(wěn)定性及進(jìn)樣精密度、日內(nèi)精密度、重復(fù)性、專屬性良好。去乙酰7-氨基頭孢烷酸、去乙酰氧7-氨基頭孢烷酸和頭孢菌素C的校正因子分別為0.80、0.82、1.67。結(jié)論此方法可以準(zhǔn)確測(cè)定7-氨基頭孢烷酸中的含量,并采用校正因子法計(jì)算有關(guān)物質(zhì)的含量。不同方法生產(chǎn)的7-氨基頭孢烷酸的含量及有關(guān)物質(zhì)無明顯差異。
[Abstract]:Objective to establish an accurate method for the determination of related substances in 7-aminocephalosporanic acid, and to determine the contents and related substances of the products produced by different methods. Methods High performance liquid chromatography was used. A C18 column (SB-C185 渭 m 脳 250mm-1) was used. The mobile phase was composed of phosphate buffer solution (5g potassium hydrogen phosphate and 5g potassium dihydrogen phosphate dissolved in 1000ml water, adjusted with phosphoric acid to 6.0-acetonitrile 922: 8) as mobile phase, the detection wavelength was 254 nm, the column temperature was 35 鈩,
本文編號(hào):1802378
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