A fingerprint of Ganoderma lucidum spore oil and its construction method and application
A technology of Ganoderma lucidum spore oil and fingerprints, which is applied to instruments, measuring devices, scientific instruments, etc., can solve the problems of insufficient rigor of results, unsuitable detection and identification, and no identification methods, and achieves reliable and effective methods and separation effects. Excellent and reproducible results
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Embodiment 1
[0056] The selection and system adaptability of embodiment 1 liquid chromatography conditions
[0057] Literature (Jin Yu. High-efficiency liquid phase fingerprint research on triterpenoids in Ganoderma lucidum spore oil [J]. Experimental research, October 2012, Volume 10, No. 29, 77-78.) and the published patent CN101435801A The mobile phase of liquid chromatography is acetonitrile-phosphoric acid (40:60, v / v), and the mobile phase conditions in the detection and identification method of the ganoderma lucidum (fruiting body) triterpenes have been disclosed. In summary, there are acetonitrile-(0.05%~0.1 %) formic acid, acetonitrile-(0.01%~0.1%) acetic acid solution, acetonitrile-water (45:55, v / v), methanol-(0.01%~1.0%) acetic acid solution, acetonitrile-0.03% phosphoric acid, acetonitrile-0.05 moL / L ammonium dihydrogen phosphate solution, methanol-0.5% perchloric acid (50:50, v / v); the elution steps have a certain ratio of isocratic and gradient.
[0058] The inventors have ...
Embodiment 2
[0075] The development research of embodiment 2 sample pretreatment method
[0076] The preparation of reference solution II refers to the extraction steps in GBT 5535.1-2008 "Determination of Unsaponifiable Matter in Animal and Vegetable Fats and Fats". Take Ganoderma lucidum spore oil, reflux for 1 hour → extract with 100ml of ether, extract 3 times respectively → wash the organic solution with water several times → Evaporate to dryness → unsaponifiable matter (triterpenes and sterol parts). This method takes a long time for pretreatment and consumes a lot of solvent.
[0077] The inventor optimizes the pretreatment method of the sample through repeated experiments, and obtains the preparation method of the test solution of the present invention, saves time, saves the amount of solvent used, and obtains the required position in the sample at the same time, and achieves the purpose. The pretreatment method Simple and economical. The reference solution II is to illustrate wh...
Embodiment 3 10
[0078] Example 3 Identification of ten batches of Ganoderma lucidum spore oil fingerprints
[0079] A total of 10 batches of Ganoderma lucidum spore oils from different origins were taken, and the test solution was prepared and detected according to the operation of Example 1 of the present invention, and the chromatogram was recorded. Intercept the spectrum at 257nm, the retention time is 50min to 97min, and the fingerprint spectrum of Ganoderma lucidum spore oil marked with peaks 1 to 13 is obtained, as figure 2 shown; the complete spectrum at 257nm is as image 3 Shown (peak numbers not marked). Depend on figure 2 As can be seen, 13 common chromatographic peaks are detected by the test product at 257nm, and the retention time of the No. 12 peak is consistent with the retention time (80.57min) of the ergosterol reference substance. 22.75min) a weak signal was observed at the peak position of the reference product. Calculate the ratio (relative retention time) of each c...
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