Test method of content of pinoresinol diglucoside in eucommia ulmoides
A technology of pinoresinol diglucoside and measurement method, which is applied in the field of chemical detection, can solve problems such as inconvenient operation, and achieve accurate measurement results
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Embodiment 1
[0024] extraction step
[0025] The equipment is ASE350 fast solvent extractor from DIONEX Company of the United States.
[0026] Step 1: Take a sample of Eucommia ulmoides, cut it into pieces, crush it, pass through a No. 3 sieve, take about 1g, weigh it accurately, add diatomaceous earth in a ratio of 1:1 by weight, mix well, and put it in a 10ml extraction pool (sample loading Add an appropriate amount of diatomaceous earth to the bottom of the extraction tank before loading, and fill the extraction tank with diatomaceous earth after loading the sample);
[0027] Step 2: First use n-hexane for static extraction, discard the n-hexane extract, continue to use methanol for static extraction, recover the methanol extract into a 50ml measuring bottle, add methanol to the mark, shake well, filter, and take the subsequent filtrate, The methanol extract is obtained;
[0028] Among them, the parameters for static extraction of n-hexane are extraction temperature 100°C, static extr...
Embodiment 2
[0039] Examination of extraction temperature
[0040] Weigh 12 samples of Eucommia ulmoides from the same batch (batch number: 140601), each about 1g, accurately weighed, and put them in the extraction pool. The static extraction time is 5 minutes, the washing volume is 100%, and the number of cycles is 2 times. Under the conditions of 80°C, 100°C, 120°C, and 140°C, four program extractions were respectively set, the extract was fixed to a 50ml volumetric flask, and samples were injected according to the chromatographic conditions described in step 3 in Example 1, and the results were calculated. See Table 1.
[0041] Table 1 Extraction temperature investigation
[0042]
[0043] It can be seen from Table 1 that the extraction efficiency is basically the same when the extraction temperature is above 100 °C. Although the viscosity of the solvent decreases with the increase of the extraction temperature, thereby enhancing the ability to dissolve the target analyte, but at th...
Embodiment 3
[0045] Investigation of static extraction time
[0046] Weigh 12 samples of Eucommia ulmoides from the same batch (batch number: 140601), each about 1g, accurately weighed, and put them in the extraction pool under the conditions that the extraction temperature is 100°C, the washing volume is 100%, and the number of cycles is 2 times. Next, set static extraction time 3min, 5min, 7min, 9min four program extractions respectively, the extract solution is settled in the 50ml measuring bottle, according to the step 3 chromatographic conditions in the embodiment 1, sample injection, calculation, the results are shown in Table 2.
[0047] Table 2 static extraction time investigation
[0048]
[0049] It can be seen from Table 2 that the extraction time is basically complete when the extraction time is 5 min. Considering saving time and solvent, the extraction time is selected as 5 min.
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