Mostafavi Ali, Abedi Ghazaleh, Jamshidi Ahmad, Afzali Daryoush, Talebi Mohammad
Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran.
Talanta. 2009 Feb 15;77(4):1415-9. doi: 10.1016/j.talanta.2008.09.024. Epub 2008 Sep 24.
A simple isocratic reversed-phase high-performance liquid chromatographic method (RP-HPLC) was developed for the simultaneous determination of buprenorphine hydrochloride, naloxone hydrochloride dihydrate and its major impurity, noroxymorphone, in pharmaceutical tablets. The chromatographic separation was achieved with 10 mmol L(-1) potassium phosphate buffer adjusted to pH 6.0 with orthophosphoric acid and acetonitrile (17:83, v/v) as mobile phase, a C-18 column, Perfectsil Target ODS3 (150 mm x 4.6mm i.d., 5 microm) kept at 35 degrees C and UV detection at 210 nm. The compounds were eluted isocratically at a flow rate of 1.0 mL min(-1). The average retention times for naloxone, noroxymorphone and buprenorphine were 2.4, 3.8 and 8.1 min, respectively. The method was validated according to the ICH guidelines. The validation characteristics included accuracy, precision, linearity, range, specificity, limit of quantitation and robustness. The calibration curves were linear (r>0.996) over the concentration range 0.22-220 microg mL(-1) for buprenorphine hydrochloride and 0.1-100 microg mL(-1) for naloxone hydrochloride dihydrate and noroxymorphone. The recoveries for all three compounds were above 96%. No spectral or chromatographic interferences from the tablet excipients were found. This method is rapid and simple, does not require any sample preparation and is suitable for routine quality control analyses.
建立了一种简单的等度反相高效液相色谱法（RP-HPLC），用于同时测定药片中的盐酸丁丙诺啡、二水合盐酸纳洛酮及其主要杂质去甲羟吗啡酮。采用10 mmol L(-1)磷酸钾缓冲液（用正磷酸调至pH 6.0）和乙腈（17:83，v/v）作为流动相，在C-18柱（Perfectsil Target ODS3，150 mm×4.6 mm内径，5 µm）上于35℃进行色谱分离，紫外检测波长为210 nm。化合物以1.0 mL min(-1)的流速等度洗脱。纳洛酮、去甲羟吗啡酮和丁丙诺啡的平均保留时间分别为2.4、3.8和8.1分钟。该方法根据ICH指南进行了验证。验证特性包括准确度、精密度、线性、范围、特异性、定量限和稳健性。盐酸丁丙诺啡在0.22 - 220 µg mL(-1)浓度范围内、二水合盐酸纳洛酮和去甲羟吗啡酮在0.1 - 100 µg mL(-1)浓度范围内的校准曲线呈线性（r>0.996）。三种化合物的回收率均高于96%。未发现片剂辅料产生的光谱或色谱干扰。该方法快速简便，无需任何样品前处理，适用于常规质量控制分析。
