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目的建立人尿液中尼非卡兰浓度测定的HPLC法,并研究健康志愿者给予注射用盐酸尼非卡兰后尼非卡兰原形经尿液的累积排泄量。方法采用内标法,以乙酸乙酯进行提取,提取液吹干,残渣用流动相溶解后进行HPLC法检测。色谱柱为μ-BondapakC_(18)(150mm×4.6mm,10μm);流动相为0.05 mol·L~(-1)磷酸二氢铵(pH 5.6)-甲醇-乙腈(60:20:20,V/V/V);流速1.0mL·min~(-1);紫外检测波长270 nm;内标为卡马西平。测定了16名健康志愿者先后给予2次负荷剂量并经连续静滴持续给药6h后,收集不同时间段的尿液样品,同时记录不同时间段的尿液体积,以测定尿药浓度后计算累积排泄量。结果尼非卡兰尿样质量浓度测定的线性范围为20～5000μg·L~(-1),最低定量限20μg·L~(-1);高、中、低3个QC(质量浓度分别为20、300和2500μg·L~(-1))的日内精密度分别为6.4%、5.8%和6.9%,日间精密度分别为8.2%、5.9%和10.9%,回收率分别为(83.0±18.9)%、(85.0±26.2)%和(74.4±4.8)%。结论该方法简便,准确,专属性强,可用于人尿液中尼非卡兰的含量测定。
OBJECTIVE To establish a HPLC method for the determination of nafcalair in human urine and to study the cumulative excretion of nifedial hydrochloride in nifediclamine hydrochloride for injection in healthy volunteers. Methods The internal standard method was used to extract with ethyl acetate. The extract was evaporated to dryness and the residue was dissolved in the mobile phase and detected by HPLC. The mobile phase consisted of 0.05 mol·L -1 ammonium dihydrogen phosphate (pH 5.6) -methanol-acetonitrile (60:20:20, V / V / V). The flow rate was 1.0 mL · min ~ (-1). The UV detection wavelength was 270 nm. The internal standard was carbamazepine. Sixteen healthy volunteers were given twice loading dose and continuous continuous infusion for 6h. The urine samples of different time periods were collected, and the urine volumes of different time periods were recorded to calculate the urine concentration Cumulative excretion. Results The linear range of nifedial in urine samples was 20 ~ 5000μg · L -1, the lowest limit of quantification was 20μg · L -1. High, medium and low 3 QC (mass concentrations were The intra-day precision of 20, 300 and 2500 μg · L -1 were 6.4%, 5.8% and 6.9%, respectively. The intra-day precision were 8.2%, 5.9% and 10.9% 18.9)%, (85.0 ± 26.2)% and (74.4 ± 4.8)%, respectively. Conclusion The method is simple, accurate and specific and can be used for the determination of nifedipine in human urine.