A kind of hplc fingerprint of hawthorn broken wall decoction pieces and its construction method and application
A technology of broken-walled decoction pieces and fingerprints, which is applied to instruments, measuring devices, scientific instruments, etc., to achieve good reproducibility, ensure stability, and shorten preparation time
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Embodiment 1
[0064] HPLC fingerprint Example 1 Pieces of broken construction method hawthorn
[0065] Pieces of broken hawthorn one kind HPLC fingerprint construction method, comprising the steps of:
[0066] S1 Preparation of test solutions: Weigh accurately hawthorn broken pieces, mass ratio of 1:25 volume of 70% methanol was added, after infiltration 12,000 rpm homogenized 2min, then cool to room temperature, made up with 70% methanol weight loss, shake, and then strained through 0.22μm filter membrane, i.e., the filtrate was the test solution;
[0067] . S2 Preparation of reference solution: chlorogenic acid as reference substance, add methanol formulated as a reference solution;
[0068] Analysis S3.HPLC chromatographic conditions: The resultant test solution through S1 octadecyl silane bonded silica column, column temperature 30 deg.] C; acetonitrile - methanol - 0.1% formic acid as the mobile phase gradient elution; flow rate It is 0.7mL / min; test solution injection volume was 20μL, t...
Embodiment 2
[0072] 2 Pieces of broken establish Hawthorn Fingerprint mode Example
[0073] 1, reference peaks identified
[0074] Construction according to the method of Example 1, the reference solution of chlorogenic acid was measured by HPLC fingerprint, record the chromatograms, and the hawthorn broken Pieces HPLC fingerprint comparison and analysis corresponding to the peak retention time and UV absorption, Such as figure 1 Indicated.
[0075] It identified: peak 4 chlorogenic acid. 6 wherein the peak height is moderate, good separation, moderate retention time, selected as the reference peak.
[0076] 2, and the establishment of common peaks of fingerprint confirmation
[0077] Take 10 Pieces of broken Hawthorn batches (batch UGP20181201, UGP20181202, UGP20181203, UGP20181204, UGP20181205, UGP20181206, UGP20181207, UGP20181208, UGP20181209, UGP20181210), prepared according to Example Construction of test solution 1, and the determination of 10 batches of test solution, record the chroma...
Embodiment 3
[0083] Example 3 embodiment of method validation
[0084] 1, specific study
[0085] Pieces of broken hawthorn batch taken UGP20180505 prepared test solution and the blank test solution, the sample S1 according to the method of Example 1, step, measured according to the chromatographic conditions of Example 1, step S3, record the chromatograms, as Figure 4 Indicated. The results show substantially no absorption in the solvent under the chromatographic conditions, little influence on the chromatogram of the sample. The method shows that the establishment of good specificity.
[0086] 2, precision instrument
[0087]The batch number of Hawthorn Broken Wall Pieces of Ugp20180505 was prepared according to the method of the first step S1, and the sample solution was prepared for 6 times, and the chromatograms were measured according to the chromatographic conditions of the first step S3 (see Figure 5 . The similarity evaluation system using the Chinese medicine chromatographic fingerpr...
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