目的 建立HPLC法测定甲磺酸双氢麦角毒碱片中4种麦角类生物碱甲磺酸双氢麦角考宁、甲磺酸双氢-α-麦角隐亭、甲磺酸双氢-β-麦角隐亭、甲磺酸双氢麦角汀。方法 使用Kromasil C₁₈色谱柱（250 mm×4.6 mm，5μm）；流动相：20 mmol/L磷酸氢二铵缓冲液（用氨试液调节pH值至8.5）–乙腈，梯度洗脱；检测波长：280 nm；柱温：35 ℃；体积流量1.0 mL/min；进样量20 μL。结果 甲磺酸双氢麦角考宁、甲磺酸双氢-α-麦角隐亭、甲磺酸双氢-β-麦角隐亭、甲磺酸双氢麦角汀均在0.05～1.00 mg/mL线性关系均良好（r＝0.999 9），平均回收率分别为101.2%、101.3%、101.3%、101.2%，RSD值分别为1.65%、1.61%、1.66%、1.64%（n＝9）。结论 建立了一种高效、准确且经济的HPLC分析方法，为甲磺酸双氢麦角毒碱片的质量控制提供更可靠的技术支撑。

Objective To establish an HPLC method to determine four ergot alkaloids dihydroergocomine mesylate, dihydro-α-ergocryptine mesylate, dihydro-β-ergocryptine mesylate, and dihydroergocristine mesylate in Dihydroergotoxine Mesylate Tablets. Methods Kromasil C₁₈chromatographic column (250 mm × 4.6 mm, 5 μm) was used with a mobile phase of 20 mmol/L ammonium phosphate (pH 8.5) - acetonitrile for gradient elution at a detection wavelength at 280 nm, column temperature set at 35 °C, flow rate of 1.0 mL/min, and injection volume of 20 μL. Results Dihydroergocomine mesylate, dihydro-α-ergocryptine mesylate, dihydro-β-ergocryptine mesylate, and dihydroergocristine mesylate had good linear relationships in the concentration range of 0.05 to 1.00 mg/mL (r = 0.999 9). Their average recovery rates were 101.2%, 101.3%, 101.3%, and 101.2%, and RSD values of 1.65%, 1.61%, 1.66%, and 1.64%, respectively (n = 9). Conclusion An efficient, accurate, and economical HPLC analysis method is established, providing more reliable technical support for the quality control of Dihydroergotoxine Mesylate Tablets.

R927.2

国家药品标准制修订研究课题（2023H032）