基于超高效液相色谱-质谱红花药材指纹图谱的建立

Establishment of Fingerprint of Safflower Based on Ultra High Performance Liquid Chromatography-Mass Spectrometry

  • 摘要: 以红花为研究对象,建立超高效液相色谱-质谱(UPLC-MS)指纹图谱分析方法,为红花药材质量鉴别提供借鉴.通过考察检测波长、梯度洗脱条件、提取溶剂、提取方法等因素,在最优条件下对20个产地的红花样品进行分离分析.色谱柱:Thermo Hypersil Gold C18,100 mm×2.1 mm,1.9 μm,流动相:0.1%甲酸水溶液(A)-乙腈(B);流速:0.3 mL/min;柱温:30℃;检测波长:270 nm;进样量:2 μL,质谱条件:鞘气流速:45 arb,辅助气流速15 arb,雾化电压:3.3 KV,离子传输管温度:350℃,辅助气加热温度:400℃.试验结果:共确定了67个共有峰,通过UPLC-MS指认了其中11个共有峰,对20批不同产地的红花药材指纹图谱进行了相似度评价,其相似度在0.687~0.971之间.建立的UPLC-MS指纹图谱可为红花药材的质量控制提供参考依据.

     

    Abstract: A Ultra high performance liquid chromatography-mass spectrometry(UPLC-MS) fingerprint analysis method was established to provide reference for the quality identification of safflower. By investigating the factors such as the detection wavelength, gradient elution condition, extraction solvent and extraction method, safflower samples from 20 producing areas were separated and analyzed under optimum conditions. Chromatographic column:Thermo Hypersil Gold C18, 100 mm×2.1 mm, 1.9 μm, mobile phase:0.1% formic acid aqueous solution (A)-acetonitrile (B); flow rate:0.3 mL/min; column temperature:30℃; detection wavelength:270 nm; injection rate:2 μL; mass spectrometry conditions:sheath gas velocity:45 arb, auxiliary gas velocity 15 arb, atomization voltage:3.3 KV, ion transfer tube temperature:350℃, auxiliary gas heating temperature:400℃. The results showed that 67 common peaks were identified and 11 of them were identified by UPLC-MS. The similarity of fingerprints of 20 batches of safflower from different habitats was evaluated. The similarity ranged from 0.687 to 0.971. The UPLC-MS fingerprint can provide the basis for the quality control of safflower.

     

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