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目的:建立同时测定复方甲硝唑克林霉素乳膏中甲硝唑、盐酸克林霉素、螺内酯、维生素B6含量的方法。方法:采用高效液相色谱法。色谱柱为Diamonsil C18,流动相为乙腈-[0.68%磷酸氢二钾溶液(含1%三乙胺)](梯度洗脱),流速为1.0 mL/min,检测波长为 210 nm,柱温为25 ℃,进样量为20 μL。结果:甲硝唑、盐酸克林霉素、螺内酯、维生素B6检测质量浓度线性范围分别为20.0~120.0 μg/mL(r=0.999 9)、10.0~60.0 μg/mL(r=0.999 1)、4.0~24.0 μg/mL(r=0.999 4)、10.0~60.0 μg/mL(r=0.999 4);定量限分别为13.06、7.36、2.43、6.42 μg/mL,检测限分别为4.18、1.82、0.76、1.79 μg/mL;精密度、稳定性、重复性试验的RSD<2.0%;回收率分别为98.97%~100.91%(RSD=0.79%,n=9)、99.02%~101.80%(RSD=1.03%,n=9)、98.18%~101.05%(RSD=1.01%,n=9)、98.75%~101.36%(RSD=0.87%,n=9)。结论:该方法简便、快速、结果准确,可用于复方甲硝唑克林霉素乳膏中甲硝唑、盐酸克林霉素、螺内酯、维生素B6含量的同时测定。
OBJECTIVE: To establish the method for simultaneous determination of the content of metronidazole, clindamycin hydrochloride, spironolactone and vitamin B6 in Compound metronidazole clindamycin cream. METHODS: HPLC method was adopted. The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-[0.68% dipotassium hydrogen phosphate solution (containing 1% triethylamine)] (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 210 nm, and column temperature was 25 ℃. The sample size was 20 μL. RESULTS: The linear ranges of metronidazole, clindamycin hydrochloride, spironolactone and vitamin B6 were respectively 20.0-120.0 μg/mL(r=0.999 9),10.0-60.0 μg/mL(r=0.999 1), 4.0-24.0 μg/mL(r=0.999 4),10.0-60.0 μg/mL (r=0.999 4). The quantitative limits were respectively 13.06, 7.36, 2.43, 6.42 μg/mL. The detection limits were 4.18, 1.82, 0.76, 1.79 μg/mL. RSDs of the precision, stability, repeatability tests were all less than 2%. The recovery rates were respectively 98.97%-100.91%(RSD=0.79%,n=9), 99.02%-101.80%(RSD=1.03%,n=9), 98.18%-101.05% (RSD=1.01%,n=9)and 98.75%-101.36%(RSD=0.87%,n=9). CONCLUSIONS: The method is simple, rapid, accurate and can be used for the determination of metronidazole, clindamycin hydrochloride, spironolactone and vitamin B6 in Compound clindamycin metronidazole cream.
甲硝唑盐酸克林霉素螺内酯维生素B6高效液相色谱法含量
MetronidazoleClindamycin hydrochlorideSpironolactoneVitamin B6HPLCContent
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