Lamiophlomis rotata medicine material, intermediate and its injection liquid finger-print atlas quality testing method
A detection method and fingerprint technology are applied in the quality detection of fingerprints of intermediates and their injections, and in the field of unique medicinal materials, which can solve the problems of not reflecting fingerprint characteristics and the like.
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Embodiment 1
[0121] Embodiment 1: The method for detecting the quality of the fingerprint spectrum of the unique medicinal material
[0122] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; flow rate: 1ml / min; detection wavelength: 254nm; column temperature: 30°C; analysis time: 1 hour; gradient elution:
[0123] gradient elution
[0124]
[0125] Preparation of the reference substance solution: take an appropriate amount of quercetin reference substance, add methanol to make a 40 μg / ml solution, and use it as the reference substance solution;
[0126] Preparation of the test solution: Take 5g of medicinal material powder that has passed through a sieve with an inner diameter of 5mm after crushing, put it in a flask, add 100ml of water, and extract by reflux for 2 hours, filter, evaporate the water to dryness, add an appropriate amount of methanol to the residue to dissolve, and centrifuge at 1000r / min , the supernatant was transf...
Embodiment 2
[0129] Embodiment 2: the fingerprint spectrum quality detection method of unique intermediate
[0130] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; flow rate: 1ml / min; detection wavelength: 254nm; column temperature: 30°C; analysis time: 1 hour; gradient elution:
[0131] gradient elution
[0132]
[0133] Preparation of the reference substance solution: take an appropriate amount of quercetin reference substance, add methanol to make a 40 μg / ml solution, and use it as the reference substance solution;
[0134] Preparation of the test solution: Take 1ml of Duyiwei injection intermediate, put it in a 10ml volumetric bottle, add 1ml of the reference solution precisely, dilute with methanol to the mark, shake well, filter with a 0.45μm microporous membrane, and take the filtrate , that is;
[0135] Assay method: draw 10 μl of the reference substance solution and the test solution, inject them into the liquid chromat...
Embodiment 3
[0137] Embodiment 3: The fingerprint spectrum quality detection method of Duyiwei Injection
[0138] Chromatographic conditions and system suitability test: use octadecylsilane bonded silica gel as filler; flow rate: 1ml / min; detection wavelength: 254nm; column temperature: 30°C; analysis time: 1 hour; gradient elution:
[0139] gradient elution
[0140]
[0141] Preparation of the reference substance solution: take an appropriate amount of quercetin reference substance, add methanol to make a 40 μg / ml solution, and use it as the reference substance solution;
[0142] Preparation of the test solution: Take 1ml of Duyiwei Injection, put it in a 10ml volumetric flask, add 1ml of the reference substance solution, dilute with methanol to the mark, shake well, filter with a 0.45μm microporous membrane, take the filtrate, and get ready;
[0143] Assay method: draw 10 μl each of the reference substance solution and the test solution, inject it into the liquid chromatograph, and m...
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