SPEHPLC法测藿香正气水中厚朴酚与和厚朴酚的含量.docVIP

SPE-HPLC法测定藿香正气水中厚朴酚与和厚朴酚的含量 摘要：建立了SPE-HPLC法测定藿香正气水中厚朴酚与和厚朴酚含量的分析方法。采用硅胶SPE小柱提取纯化样品。色谱柱：C18（250 mm×4.6 mm I.D.，5 μm），以甲醇-水-乙腈-冰醋酸（70∶25∶5∶0.25）为流动相，流速为1.0 mL·min-1，检测波长为294 nm，柱温为室温。SPE~HPLC法测得厚朴酚浓度在4.0-80 μg·mL-1 (r=0.9998)，和厚朴酚浓度在2.0~40 μg·mL-1 (r=0.9998) 范围内与其峰面积线性关系良好。厚朴酚的平均回收率为99.8%，RSD为0.8%，和厚朴酚的平均回收率为99.6%，RSD为0.5%。该方法快速、简便、准确、重现性好，能有效地控制藿香正气水的质量。 关键词：SPE HPLC 藿香正气水 厚朴酚 和厚朴酚 Determination of Magnolol and Honokiol in Huoxiangzhengqi Water by SPE-HPLC Abstract: A SPE-HPLC method for determining the contents of Magnolol and Honokiol in Huoxiangzhengqi Water was established. Samples were purified by silica gel SPE column. The HPLC column used in the experiment was C18 （250 mm×4.6 mm I.D., 5 μm）, and the mobile phase was methanol-water-acetonitrile-acetic acid (70: 25: 5: 0.25). The flow rate of the mobile phase was 1.0 mL·min-1 and detection wavelength was 294 nm. The experiment was accomplished at room temperature. It had good linear relationship between the peak areas of Magnolol and Honokiol and their concentrations at 4.0-80.0 μg·mL-1 (r=0.9998), 2.0-40.0 μg·mL-1 (r=0.9998), respectively. The average recovery of Honokiol was 99.6% with RSD being 0.5%, and that of Magnolol was 99.8% with RSD being 0.8%. The method was rapid, simple, accurate, with good reproducibility, and it can be used for quality control of Huoxiangzhengqi Water. Key words: SPE HPLC Huoxiangzhengqi Water Magnolol Honokiol 藿香正气水系由甘草、陈皮、厚朴等多味中药制成的传统中成药，功能解表化湿、理气和中，常用于外感风寒、内伤湿滞或夏伤暑湿所致的感冒[1]，具有抗菌、抗病毒、抗过敏、影响胃肠活动、肌肉松弛和中枢抑制等作用[2]。《中国药典》2005年版一部[1]中以厚朴酚与和厚朴酚的含量作为藿香正气水的质量控制指标，以氯仿为溶剂，采用液液萃取技术对样品进行预处理，然后以高效液相色谱法(HPLC)进行含量测定。但液-液萃取预处理技术费时、易乳化、需要样品量大,并且需要较多有毒或有污染的有机溶剂，易污染环境。而采用固相萃取技术（SPE）可以避免上述缺点。固相萃取具有高的回收率和富集倍数，还具有有机溶剂用量少，无相分离操作可避免产生乳化，分析物流分易于收集，能处理小体积试样，操作简单快速等优点[3-5]。文献[6, 7]采用高效液相色谱法测定了藿香正气水中厚朴酚与和厚朴酚的含量，采用直接稀释法对样品进行前处理。此外，还有对藿香正气水中白芷、橙皮苷、甘草苷、水合氧化前胡素、花椒毒素、甘草酸、橙黄酮或异橙黄酮、欧前胡素等的研究[8-11]。本文在药典方法的基础上，建立了采用SPE样品预处理技术纯化样品，再利用HPLC法对厚朴酚与和厚朴酚进行定量分析，并进行了系统的方法学考察，评价SPE技术用于该药品预处理的实用性。 1实验部分 1.1 仪器与试药 1.