Xiaojin pill fingerprint detection method
A detection method and fingerprint technology, which is applied in the detection field of Xiaojin Pill fingerprints, can solve problems such as control, complex composition of medicinal flavors, and difficult overall quality of Xiaojin Pills, so as to achieve overall control, improve the quality evaluation system, and ensure the effect of clinical curative effect
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Embodiment 1
[0034] Embodiment 1 Fingerprint detection of fat-soluble parts of Xiaojin Pills of the present invention
[0035] 1) Preparation of the test product solution in the fat-soluble part: take Xiaojin pills and crush them into fine powder, weigh 0.6g precisely, add 5mL ether, ultrasonicate for 30min, filter, add 3mL ether to the filter residue, ultrasonically 15min, filter, wash the filter residue with 2mL ether, and combine the filtrates , evaporate the solvent at 40°C, add methanol to dissolve the residue, dilute the methanol to 5mL, pass through a 0.22μm filter membrane, and obtain the product;
[0036] 2) draw need testing solution and inject high-performance liquid chromatograph, and chromatographic condition is as follows:
[0037] Chromatographic column: Welch UltiMate AQ-C18 (4.6×250mm); detection wavelength: 202nm; injection volume is 15ul, flow rate is 1ml / min, column temperature is 30°C; mobile phase: acetonitrile as mobile phase A, 0.1% Phosphoric acid solution is mobi...
Embodiment 2
[0041] Embodiment 2 Fingerprint detection of water-soluble parts of Xiaojin pills of the present invention
[0042] 1) Preparation of the water-soluble part of the test solution: take the filter residue of step 2) of Example 1, evaporate the residual ether, add 5 times the amount (v / w; mL / g) of 70% ethanol, ultrasonic 30min, centrifuge, take the The clear liquid was passed through a 0.22 μm filter membrane;
[0043] 2) Draw the water-soluble part for the test product solution and inject it into the high-performance liquid chromatograph, and the chromatographic conditions are as follows:
[0044] Chromatographic column: chromatographic column is Welch UltiMate AQ-C18 (4.6×250mm); detection wavelength: 250nm; injection volume is 15ul, flow rate is 1ml / min, column temperature is 30°C; mobile phase: acetonitrile as mobile phase A, Use 0.1% phosphoric acid solution as mobile phase B; the gradient elution procedure is as follows:
[0045]
[0046]
[0047] 3) The fingerprints ...
experiment example 1
[0050] 1. Instrument
[0051] Thermo Scientific UltiMate 3000 high-performance liquid chromatography, Welch UltiMate AQ-C18 chromatographic column (4.6 × 250mm).
[0052] 2. Reagents
[0053] Chromatographic acetonitrile, UP ultrapure water, phosphoric acid, ether, chromatographic grade methanol, pure ethanol.
[0054] 3. Liquid chromatography system conditions
[0055] Gradient elution is adopted, the mobile phase A is 0.1% phosphoric acid aqueous solution, the mobile phase B is acetonitrile, the elution time of the fat-soluble part is 80 minutes, the elution time of the water-soluble part is 58 minutes, and the flow rate is 1.0ml / min; the column temperature is 30 °C; The ultraviolet detection wavelength of the soluble part is 202nm, and the ultraviolet detection wavelength of the water-soluble part is 250nm;
[0056] Gradient elution program for fat-soluble parts: 0-5min, 40% acetonitrile; 5-10min, 40%-50% acetonitrile; 10-20min, 50%-60% acetonitrile; 20-30min, 60%-65% ac...
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