HPLC-DAD同时测定清感穿心莲片中3种成分的含量

Simultaneous Determination of Three Components in Qinggan Chuanxinlian Tablet by HPLC-DAD

关键词:  清感穿心莲片  穿心莲内酯  脱水穿心莲内酯  异丹叶大黄素  多成分测定  质量控制

Key words:  Qinggan Chuanxinlian tablet  andrographolide  dehydroandrographolide  isorhapontigenin  multicomponent determination  quality control

摘要:

目的 建立清感穿心莲片中穿心莲内酯、脱水穿心莲内酯和异丹叶大黄素3种成分的HPLC含量测定方法，为清感穿心莲片的质量控制提供参考。方法 采用HPLC-DAD法，Agilent Extend C₁₈色谱柱（4.6 mm×250 mm，5 μm），以乙腈（A）-水（B）为流动相进行梯度洗脱，检测波长225 nm （穿心莲内酯），254 nm （脱水穿心莲内酯），323 nm （异丹叶大黄素），柱温35℃，流速0.8 mL·min^-1。结果 穿心莲内酯、脱水穿心莲内酯和异丹叶大黄素分别在8.395~335.790 μg·mL^-1（r=0.999 9），5.948~237.924 μg·mL^-1（r=0.999 9）和0.854~25.607 μg·mL^-1（r=0.999 9）内线性关系良好；平均加样回收率分别为97.2%，102.1%和98.2%，RSD分别为1.7%，3.0%和1.0%。对来自2个企业的14批次样品进行测定，穿心莲内酯、脱水穿心莲内酯和异丹叶大黄素含量范围分别为每片0.80~2.43，0.59~2.71，和0.045~0.275 mg。结论 本方法准确可靠，可用于清感穿心莲片的质量控制。

Abstract:

OBJECTIVE To establish an HPLC method for simultaneous determination of andrographolide, dehydroandrographolide and isorhapontigenin in Qinggan Chuanxinlian tablet, and to provide the evidence for its quality control. METHODS The HPLC-DAD analysis was carried out by Agilent Extend C₁₈ column (4.6 mm×250 mm, 5 μm) with acetonitrile(A)-water solution(B) as the mobile phase for gradient elution. The detection wavelength was 225 nm for andrographolide, 254 nm for dehydroandrographolide, and 323 nm for isorhapontigenin, respectively. In addition, the column temperature was 35, and the flow rate was 0.8℃ mL·min^-1. RESULTS The linear range was 8.395-335.790 μg·mL^-1 for andrographolide(r=0.999 9), 5.948-237.924 μg·mL^-1 for dehydroandrographolide(r=0.999 9) and 0.854-25.607 μg·mL^-1 for isorhapontigenin(r=0.999 9); the average recoveries were 97.2%, 102.1% and 98.2%, and RSD were 1.7%, 3.0%, 1.0%, respectively. The contents of three components in 14 batches from 2 manufactories were 0.80-2.43, 0.59-2.71, and 0.045-0.275 mg per tablet. CONCLUSION This method is accurate and reliable, and it is suitable for the quality control of Qinggan Chuanxinlian tablet.