Department of Preventive and Social Dentistry, Graduate School, Kyung Hee University, Hoegi-dong, Dongdaemoon-gu, Seoul 130-701, South Korea.
J Pharm Biomed Anal. 2011 Jan 5;54(1):217-21. doi: 10.1016/j.jpba.2010.07.037. Epub 2010 Aug 6.
We developed a highly sensitive and selective reversed-phase HPLC-pulsed amperometric detection (RP-HPLC-PAD) method for cardiac glycoside detection. Eight cardiac glycosides were completely separated within 45 min on a reversed-phase column using a water-acetonitrile gradient, and were detected using a PAD under NaOH alkaline conditions. The detection (S/N=3) and quantification (S/N=10) limits for the cardiac glycosides were 0.1-0.3 and 0.3-0.8 ng, respectively. The linear regression coefficient was 0.9962-0.9998 for concentrations of 1-25 μg/mL. Cardiac glycosides in the Digitalis purpurea leaf displayed intra- and inter-day precisions (RSDs) of <9.30% and average recoveries of 98.63-99.94%. The contents of gitoxin, digitonin, and digitoxin in the D. purpurea were 0.197, 0.11, and 0.379 mg/g for leaf dried at 60 °C, 0.058, 0.11, and 0.090 mg/g for leaf dried at ambient temperature, and N.D. (not detected), and 18.379 mg/g, N.D. for seed, respectively. We conclude that our method shows good precision and accuracy.
我们开发了一种高灵敏度和选择性的反相高效液相色谱-脉冲安培检测（RP-HPLC-PAD）方法，用于检测强心苷。八种强心苷在反相柱上用乙腈-水梯度洗脱，在 NaOH 碱性条件下用 PAD 检测，可在 45 分钟内完全分离。强心苷的检测（S/N=3）和定量（S/N=10）限分别为 0.1-0.3 和 0.3-0.8 ng。浓度为 1-25 μg/mL 时，线性回归系数为 0.9962-0.9998。毛地黄叶片中的强心苷在日内和日间精密度（RSDs）<9.30%，平均回收率为 98.63-99.94%。在 60°C 干燥的毛地黄叶中，毛地黄苷、地高辛和地高辛的含量分别为 0.197、0.11 和 0.379 mg/g，在室温下干燥的毛地黄叶中，分别为 0.058、0.11 和 0.090 mg/g，种子中未检出（N.D.），地高辛含量为 18.379 mg/g，N.D.。我们得出结论，我们的方法显示出良好的精密度和准确性。
