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目的:同时测定道地产补骨脂-肉豆蔻药对中7个指标成分含量,并对其化学成分进行初步归属和鉴定。方法:高效液相色谱法测定条件:Waters Acquity UPLC BEH C18色谱柱(100 mm×2.1 mm,1.7μm);流动相为乙腈-水,梯度洗脱;流速0.25 m L/min;进样量2μL;柱温30℃;检测波长254 nm。液质联用法测定条件:Waters HSS T3色谱柱(100 mm×2.1 mm,1.7μm),采用电喷雾电离离子源;正离子模式检测:m/z 500~1 200,毛细管电压为3.0k V;锥孔电压为22 k V;离子源温度为110℃;脱溶剂温度为450℃;脱溶剂气体流速为800 L/h;锥孔气流量50 L/h。结果:各指标成分在选定的浓度范围内线性关系良好,加样回收率为95.07%~98.16%,RSD为1.23%~1.97%。结论:该试验为道地产补骨脂-肉豆蔻药对的质量控制和深入研究奠定了基础。
OBJECTIVE: To determine the content of 7 index components in the real estate psoralen-nutmeg medicine at the same time, and initially identify and identify its chemical components. METHODS: The HPLC conditions were as follows: Waters Acquity UPLC BEH C18 column (100 mm × 2.1 mm, 1.7 μm); mobile phase consisted of acetonitrile-water with gradient elution; flow rate of 0.25 mL / min; injection volume of 2 μL ; Column temperature 30 ℃; detection wavelength 254 nm. The conditions for the determination of LC-MS were: Waters HSS T3 column (100 mm × 2.1 mm, 1.7 μm) with electrospray ionization ion source; positive ion mode detection: m / z 500-1 200; capillary voltage 3.0 k V; Cone hole voltage of 22 kV; Ion source temperature of 110 ℃; Desolvation temperature of 450 ℃; Desolvation gas flow rate of 800 L / h; Cone flow of 50 L / h. Results: The linearity of each index was within the range of the selected concentration. The recoveries were 95.07% -98.16% with RSDs of 1.23% -1.97%. Conclusion: This test lays the foundation for the quality control and in-depth study of the real estate psoralen-nutmeg medicine.