Ophiopogon japonicus fingerprint, its construction method and quality detection method of Ophiopogon japonicus
A technology of fingerprint spectrum and construction method, applied in the field of drug testing, can solve the problems of single quality evaluation method of Ophiopogon japonicus, indicating the overall quality of Ophiopogon japonicus and its preparation, etc., and achieve stable retention time, no drift, and good reproducibility. Effect
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Embodiment 1
[0077] The present embodiment provides a kind of Radix Ophiopogon japonicus fingerprint, and it comprises the following steps to construct:
[0078] Prepare the test solution: accurately weigh 2.0g of Ophiopogon japonicus, dry and crush it; put it in a stoppered conical flask, add 15 times the volume of water, weigh, decoct for 2 hours, cool, add weight, and filter to get the test product solution.
[0079] Preparation of reference substance solution: Accurately weigh an appropriate amount of uridine reference substance, and use 5% aqueous methanol to prepare a solution containing 50 μg of uridine per 1 ml.
[0080] HPLC analysis
[0081] According to high performance liquid chromatography (2015 edition " Chinese Pharmacopoeia " three general rules 0512) test.
[0082] Chromatographic conditions: chromatographic column is Wters Bridge (5μm, 4.6×250mm Column); mobile phase: A: acetonitrile; B: 0.058% trifluoroacetic acid; gradient elution; column temperature: 40°C; detection ...
Embodiment 2
[0097] One of the differences between Example 2 and Example 1 is that the test solution used in Example 2 is different. In Example 2, the test solution is prepared from the Shengmai injection of WS3-B-2865-98-2011 Craft made.
[0098] Using the traditional Chinese medicine chromatographic fingerprint similarity evaluation system to analyze the detection results of the fingerprints of 11 batches of test products, and generate a control fingerprint; through the identification and identification of the characteristic peaks, 6 characteristic peaks of the HPLC fingerprint of the intermediate product of Ophiopogon japonicus were obtained , fingerprints such as figure 2 As shown, with No. 2 peak uridine as the reference peak, the relative retention time of each characteristic peak is: No. 1 peak: relative retention time is 0.859-0.868; relative peak area is 0.434-0.517; No. 2 peak: relative retention time is 1; relative peak area is 1; No. 3 peak: relative retention time is 1.235-1...
Embodiment 3
[0104] One of the differences between Example 3 and Example 1 is that the chromatographic conditions are different. The chromatographic conditions are as follows: select octadecylsilane bonded silica gel as a chromatographic column as a filler, use acetonitrile as mobile phase A, and use 0.06vol% trifluoroacetic acid aqueous solution as mobile phase B to compare the reference substance solution and the test solution respectively Gradient elution was carried out, and during the gradient elution process, the column temperature was controlled at 42° C., the flow rate was 0.61 mL / min; the detection wavelength was 278 nm.
[0105] Two of the difference between embodiment 3 and embodiment 1 is that the reference substance solution is different;
[0106] Reference substance solution: the solvent is 5vol% methanol aqueous solution, the solute is uridine, and the uridine concentration is 51 μg / ml.
[0107] The third difference between embodiment 3 and embodiment 1 is that the preparat...
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Abstract
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