A method of one test and multiple evaluations for different grades of Alisma and its application
A technology of grade and Alisma, applied in the field of one-test and multiple-evaluation methods, can solve problems such as difficult to reflect the overall quality of Alisma, difficult to separate and prepare, difficult to obtain, etc., to achieve good application prospects, fast and accurate methods, and high reproducibility Effect
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[0045] 1.3 Preparation of solution
[0046] 1.3.1 Preparation of mixed reference solution
[0047] Accurately weigh the reference substances of epoxy alisene, 23-acetyl alisol C, alis alcohol A, alis enol, alis alcohol B, 23-acetyl alisol B and 11-deoxy alisol B Appropriate amount was added to acetonitrile for ultrasonic dissolution to prepare single reference substance stock solutions with mass concentrations of 1.020, 1.021, 0.436, 1.005, 0.966, 1.130 and 0.858 mg·mL-1, respectively, for future use. Accurately measure the appropriate amount of the above-mentioned reference substance solution respectively, put them in the same volumetric flask, add 50% acetonitrile to the mark, and obtain 20.40 μg·mL-1 of epoxy alisene, 20.1 μg·mL-1 of 23-acetyl alisolol , alisol A 109.0μg·mL-1, alisolenol 100.5μg·mL-1, alisol B 241.5μg·mL-1, 23-acetyl alisol B 141.3μg·mL-1 and 11- Deoxyalisol B17 1.6 μg·mL-1 mixed reference solution.
[0048] 1.3.2 Preparation of the test solution
[004...
Embodiment 1
[0109] A method of one test and multiple evaluations for different grades of Alisma, comprising the following steps:
[0110] (1) Take 130 batches of Alisma samples from S66-S195, grind them into powder respectively, pass through an 80-mesh sieve, and then place 1.0 g of them into a corked Erlenmeyer flask, accurately add 25 ml of acetonitrile, seal them tightly, and weigh them , sonicated for 30 minutes (power 250W, frequency 50kHz), let cool, weighed again, supplemented with acetonitrile to reduce weight loss, shake well, the extract was centrifuged at 10 000r min-1 for 10min, filtered through a 0.22μm filter membrane, and the filtrate was taken. Obtain the test solution;
[0111] (2) use ultra-high performance liquid chromatography to measure the content of 23-acetylalisol B in need testing solution according to the following conditions;
[0112] The conditions are: chromatographic column: Waters CORTECS C18 column (2.1mm×100mm, 1.6μm); mobile phase is water (A)-acetonitri...
Embodiment 2
[0124] A method of one test and multiple evaluations for different grades of Alisma, comprising the following steps:
[0125] (1) Take Alisma sample, grind it into powder, pass it through an 80-mesh sieve, then place it into a precise 1.0g Erlenmeyer flask with a stopper, precisely add 25ml mL of acetonitrile, seal it tightly, weigh it, and ultrasonically treat it for 30min (power 250W , frequency 50kHz), let cool, weighed again, supplemented with acetonitrile to reduce weight loss, shake well, the extract was centrifuged at 10000r min-1 for 10min, filtered through a 0.22μm filter membrane, and the filtrate was taken to obtain the test solution;
[0126] (2) use ultra-high performance liquid chromatography to measure the content of 23-acetylalisol B in the need testing solution according to the following conditions;
[0127] The conditions are: chromatographic column: Waters CORTECS C18 column (2.1mm×100mm, 1.6μm); mobile phase is water (A)-acetonitrile (B), gradient elution: ...
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