Characteristic chromatogram of ground beetle water extract and preparation thereof and construction method of characteristic chromatogram
A construction method and water extract technology, applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of less characteristic peaks, poor separation effect, unsuitable quality detection, etc., and achieve good peak shape, stable baseline and effective quality detection Effect
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experiment example 1
[0054] Investigation of the Construction Method of Experimental Example 1
[0055] 1. Instruments, reagents and reagents
[0056] Instrument: Shimadzu LC-20AD HPLC: PDA detector, Labsolutions chromatographic workstation; Thermo Fisherman Thermo U3000, Chromeleon7 chromatographic workstation; XP26 (Mettler-Toledo), BSA124S electronic balance (Sartorius Scientific Instruments (Beijing) Co., Ltd.), BT25S electronic balance (Sartorius Technology Instrument (Beijing) Co., Ltd.), KQ-500DB ultrasonic cleaner (Kunshan Ultrasonic Instrument Co., Ltd.).
[0057] Chromatographic column: Venusil HILIC (4.6×150mm, 5μm), Waters Atlantis HILIC Silica (4.6*150mm, 5μm).
[0058] Reagent: Wood Beetle Formula Granules can be prepared by conventional methods in the art. For example, in the present invention, it is prepared according to the following steps: take 200 kg of decoction pieces of soil beetle, extract once by boiling (100° C.), and add 12 times the amount of decoction pieces (add water...
experiment example 2
[0141] Experimental Example 2 Methodological Verification
[0142] 1. Repeatability
[0143] Take 6 parts of the ground beetle formula granules (batch number: 20030752), measure according to the method of Example 1, obtain its characteristic spectrum, and take No. 5 peak as the reference peak, calculate its relative peak area and relative retention time. And calculate the RSD. The result is shown below.
[0144] Table 16 Retention time and relative retention time table for the repeatability investigation of characteristic chromatograms
[0145]
[0146] Table 17 Characteristic spectrum repeatability investigation peak area and relative peak area
[0147]
[0148]
[0149] Summary: According to the repeatability investigation results, the relative retention time RSD of each characteristic peak is 0% to 0.8%, and the relative peak area RSD is in the range of 0% to 1.8%, indicating that the characteristic spectrum has good repeatability.
[0150] 2. Intermediate precis...
Embodiment 1
[0179] This embodiment provides a method for constructing a characteristic map of wood beetle formula particles, including the following steps:
[0180] Preparation of the test solution: get an appropriate amount of this product, grind it finely, get about 0.3g, accurately weigh, put in a stoppered Erlenmeyer flask, add 25ml of 30% methanol accurately, weigh, ultrasonically process (power 250W, frequency 40kHz) for 30 minutes, let cool, weigh again, make up the lost weight with 30% methanol, shake well, filter, and take the filtrate to obtain the final product.
[0181] Preparation of reference substance solution: Take an appropriate amount of hypoxanthine reference substance, accurately weigh it, add 30% methanol to make a reference substance solution containing 10 μg per 1 ml, and use it as the reference substance reference solution.
[0182] Each 2 μ l of the above-mentioned ground beetle formula granule need testing solution and reference substance solution is injected int...
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