摘要
建立了高效液相色谱-荧光法同时测定红霉素、甲红霉素、罗红霉素的方法.该方法以9-芴代甲氧苯酰氯（FMOC-CL）为衍生试剂,以V（乙腈）：V（磷酸二氢钾）=3：1为反应体系,于50℃反应1 h.液相色谱分析条件为：ExtendC18柱（4.6 mm i.d.×150 mm）,乙腈-25 mmoL磷酸二氢胺（pH 7）为流动相,梯度淋洗;柱温30℃,流速1.5 mL/min,激发波长255 nm、发射波长315 nm.线性范围分别为红霉素0.5～100μg、甲红霉素0.5～100μg、罗红素0.1～150μg.检出限为红霉素1μg/mL、甲红霉素1μg/mL、罗红霉素0.25μg/mL.加标回收率为90%～97%,相对标准偏差为3.5%～7.9%.
A method was established for the detection of erythromycin, clarithromycin and roxithromycin by high-perforrnance liquid chromatography with fluorometric detection. FMOC-CL used as derivation reagent and acetonitrile KH2 PO4 used as reaction system, at 50 ℃ reacted for 1 h. The chromatographic conditions were as follows, column： Extend-C18（4.6 mm i.d.× 150 mm） ; mobile phase ： acetonitrile-25 mmoL NH4 H2 PO4 （ gradient elution） ; column temperature： 30 ℃ ; flow rate： 1.5 mL/min; detection wavelength： excitation wavelength 255 nm and emission wave- length 315 nm. The linear range were 0.5 ～ 100μg for erythromycin, 0.5 ～100μg for clarithromycin and 0.1～ 150 μg for roxithromycin. The detection limits were 1 μg/mL for erythromycin, 1 μg/mL for clarithromycin and 0.25μg/mL for roxithromycin. The recoveries of erythromycin, clarithromycin and roxithromyein were 97.9 %, 90.7 %, 93.6 % with relative standard deviations of 3.5 %～7.9%.
出处
《分析试验室》
CAS
CSCD
北大核心
2006年第6期63-66,共4页
Chinese Journal of Analysis Laboratory
