Characteristic chromatogram of chingma abutilon seed and preparation thereof, construction method of characteristic chromatogram and content determination method
A construction method and technology of characteristic map, which are applied in the field of characteristic maps of Mallow seeds and their preparations, their construction methods and content determination, can solve the problems of low resolution of characteristic maps, few characteristic peaks and the like, and achieve reproducibility. Good results with high accuracy and low limit of quantitation
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experiment example 1
[0084] 1. Instruments and reagents:
[0085] Instrument: Waters ACQUITY H-Class ultra-high performance liquid chromatograph, PDA detector (Waters Corporation), TUV Detector ultraviolet detector, Empower 3 chromatography workstation; ML204T electronic balance (Mettler Toledo); MSA6.6S-0CE-DI electronic Balance (Sardoris); JJ500 electronic balance (Changshu Shuangjie Testing Instrument Factory); KQ-300DE Ultrasonic Cleaner (Kunshan Ultrasonic Instrument Co., Ltd.).
[0086] Column: ACQUITY BEH Shield RP18 (2.1×100mm, 1.7μm);
[0087] Test drug: caffeic acid reference substance (batch number: 110885-201703, China National Institute for Food and Drug Control). Methanol, acetonitrile (MERCK) and phosphoric acid (Thermo Fisher Scientific) were of chromatographic grade; water was distilled water (Watson's); other reagents were of analytical grade.
[0088] Mallow seeds are commercially available.
[0089] The preparation method of the standard decoction freeze-dried powder of Ma...
experiment example 2
[0123] Experimental example 2 Methodological verification
[0124] 1. Precision
[0125] (1) Repeatability
[0126] Take 6 parts of mallow seed formula granules (batch number: 20030431), prepare the test solution according to the method under item 2 of experimental example 1 and measure, obtain its characteristic spectrum, take the peak of No. 2 as the reference peak, calculate No. 1 to No. 8 Relative retention times of characteristic peaks. And calculate the RSD, the results are shown in the table below.
[0127] Table 5 Mallow seed formula granules repeatability investigation retention time and relative retention timetable
[0128]
[0129] The results of the repeatability experiment show that the relative retention time RSD of each characteristic peak is in the range of 0.08% to 0.35% except that the relative retention time RSD of peak 2 is 0 in the six repeatable experimental samples, indicating that the characteristic peaks of the characteristic map are repeated. S...
experiment example 3
[0152] The investigation of the chromatographic conditions in the experimental example 3 content determination method
[0153] 1. Instruments and reagents
[0154] The same as in Experimental Example 1.
[0155] 2. Test method for caffeic acid content in mallow seed preparations
[0156] (1) Preparation of reference substance solution: take an appropriate amount of caffeic acid reference substance, accurately weigh it, add 10% by volume methanol aqueous solution to prepare a reference substance solution containing 30 μg of caffeic acid per 1ml;
[0157] (2) preparation of the test solution: take the decoction pieces of the mallow seed, the standard decoction freeze-dried powder of the mallow seed or the formula granules of the mallow seed as the test product to prepare the respective test solution, the concrete method is as follows: Appropriate amount of the product, grind finely, take about 0.5g, accurately weigh it, put it in a conical flask with a stopper, accurately add ...
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