A kind of citrus citrus medicinal material fingerprint, its establishment method and application
A method for establishing and fingerprinting technology, which are applied in the identification of the quality of Citrus aurantium medicinal materials (whether it is qualified or not), the high performance liquid chromatography (HPLC) fingerprint of Citrus Citrus medicinal materials and its establishment, identification of Citrus Citrus medicinal materials, and the fields of fingerprints of Citrus Citrus medicinal materials, It can solve the problems that cannot fully reflect the type and quantity of internal chemical components of traditional Chinese medicine, and the method for determining the content of synephrine is complex, and achieves good stability and reproducibility.
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Embodiment 1
[0056] Example 1: Establishment and verification of HPLC fingerprints of Citrus aurantium medicinal material
[0057] 1. Instruments and reagents
[0058] Shimadzu (SHIMADZU) LC20A high performance liquid chromatograph, equipped with LC-20AT binary pump, SPD-M20A diode array detector, CTO-20A column thermostat and SIL-20AC autosampler, LCsolution chromatography workstation management software and online degasser.
[0059] Water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure.
[0060] The 8 batches of Citrus aurantium medicinal materials were all purchased from genuine medicinal materials in regular pharmacies (attached with test reports according to the Pharmacopoeia).
[0061] 2. Establishment of HPLC fingerprints of Citrus aurantium medicinal material
[0062] 2.1 Preparation of the test solution: Weigh 10 g of the first batch of Citrus aurantium medicinal material, add 100 mL of distilled water to reflux for ...
Embodiment 2
[0078] Example 2: Qualitative identification of characteristic peaks in the HPLC fingerprint of Citrus aurantium medicinal material
[0079] 1. Instruments and reagents: Aglient1100 liquid chromatograph; Aglient6300IonTrap mass spectrometer; water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure; medicinal materials are purchased from regular pharmacies.
[0080] 2. Chromatography and mass spectrometry conditions: AgilentTC-C column packing 18 , the specification is 250mm×4.6mm, 5μm; the mobile phase is acetonitrile-water (containing 0.1% formic acid) gradient elution; the gradient elution conditions are: 0min→20min→45min→60min→75min→77min, acetonitrile 3%→20% →20%→30%→80%→100%; flow rate 1.0mL / min; column temperature 30°C; injection volume 5μL; ion source is ESI, scan in negative ion mode, nebulizer pressure is 40psi, dryer flow rate is 10.0L / min, the ion source temperature is 350°C, and the mass scan range is 200-...
Embodiment 3
[0087] Example 3: Application of Standard Fingerprint Spectrum in Identifying Citrus Aurantium Medicinal Material
[0088] 1. Instruments and reagents
[0089] Shimadzu (SHIMADZU) LC20A high performance liquid chromatograph, equipped with LC-20AT binary pump, SPD-M20A diode array detector, CTO-20A column thermostat and SIL-20AC autosampler, LCsolution chromatography workstation management software and online degasser.
[0090] Water is pure water; methanol and acetonitrile are chromatographically pure; other reagents are analytically pure.
[0091] The medicinal materials of Fructus Aurantii to be tested were randomly purchased; the standard sample was the first batch of Fructus Aurantii medicinal materials in Example 1.
[0092] 2. Determination of HPLC fingerprints of Citrus aurantium medicinal material
[0093] 2.1 Preparation of the test solution: Weigh 10 g of Citrus aurantii medicinal material, add 100 mL of distilled water to reflux for extraction twice, each time fo...
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