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目的建立一种快速、准确测定人血浆中盐酸二甲双胍含量的反相离子对HPLC方法。方法在血浆中加入盐酸二甲双胍标样及内标阿替洛尔,用乙腈除蛋白,离心后取上清液加二氯甲烷萃取乙腈,再次离心后,取上清液直接进样分析;色谱柱为Diamonsil C18(150×4.6 mm,5μm),流动相组成:(0.01mol/L磷酸二氢钠+0.007 5mol/L十二烷基磺酸钠)(pH 5.5):乙腈(70∶30),检测波长为235 nm,柱温:30℃,流速为1.0mL/min,进样量为20μL。结果盐酸二甲双胍在0.05~4μg/mL的浓度范围内呈良好线性,r=0.999 7,最低检测限为0.015μg/mL,方法回收率大于97.98%,萃取回收率大于89.35%,日间、日内变异系数均小于5%。结论该方法准确、快速、灵敏,可用于盐酸二甲双胍的治疗药物监测、人体内药代动力学及生物等效性研究。
OBJECTIVE To establish a rapid and accurate RP-HPLC method for the determination of metformin hydrochloride in human plasma. Methods Plasma samples were treated with metformin hydrochloride and atenolol internal standard, deproteinized with acetonitrile, centrifuged, and the supernatant was extracted with methylene chloride to extract acetonitrile. After centrifugation again, the supernatant was directly injected into the column for analysis. Column (150 × 4.6 mm, 5 μm). The mobile phase consisted of (0.01 mol / L sodium dihydrogenphosphate + 0.007 5 mol / L sodium dodecyl sulfate) (pH 5.5): acetonitrile The detection wavelength was 235 nm, the column temperature was 30 ℃, the flow rate was 1.0 mL / min and the injection volume was 20 μL. Results Metformin hydrochloride showed a good linearity within the range of 0.05-4 μg / mL with r = 0.999 7 and the lowest limit of detection was 0.015 μg / mL. The recovery was greater than 97.98% and the extraction recovery was more than 89.35% Coefficients are less than 5%. Conclusion The method is accurate, rapid and sensitive and can be used for the monitoring of methotrexate hydrochloride, pharmacokinetics and bioequivalence in human body.