Original celastrus angulatus medicine as well as preparation method and mass detection method thereof
A quality detection method, the technology of paretin, which is applied in the field of botanical pesticides and can solve the problems of fingerprint detection that have not been reported.
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[0127] ④ Preparation of the test solution
[0128] Accurately weigh 200mg of 15% T12 phasanthalin or 2% phasanthalin water suspension in a 100mL volumetric flask, add an appropriate amount of methanol to dissolve, dilute to the mark after ultrasonic oscillation, and shake well to obtain 15% photericin Rattan original drug or 2% phaelopedin aqueous suspension for the test solution.
[0129] ⑤Measurement of precision
[0130] The test solution was repeatedly injected 5 times, the relative standard deviation of the peak area was RSD=1.02%, and the relative standard deviation of the retention time was RSD=0.45%.
[0131] ⑥ Determination of the test product
[0132] Draw each test product solution, inject sample, measure its peak area, and obtain the content of picrocetin B.
[0133] ⑦Determination of recovery rate
[0134] Using the standard addition method, 100 μg / mL was added to the test product of phareidin original drug, and the average recovery rate was 103.5%.
[0135] ...
Embodiment 1
[0264] (1) Preparation method of 15% T12 picrodermin original drug A
[0265] After sieving, the vine root or / and skin (24 mesh) of Shaanxi Baoji bitter bark that meets the requirements is sequentially added with ethanol with a volume of 3︰2︰2 times the amount (mass ratio) of 95% (mass ratio), and refluxed at 80°C for 2 hours (extraction 3 times, 2h each time), filter, combine the three filtrates, and concentrate under reduced pressure to a filtrate with a density of 1.08. Take this filtrate, add 1 times its volume of precipitant (10% ethanol by mass ratio), precipitate for 12 hours, and centrifuge to obtain the precipitate, that is, 15% T12 phalaetanin original drug A.
[0266]
[0267] (2) Quality testing method of 15%T12 picratine original drug A
[0268] ①Preparation of characteristic extracts
[0269] Take 1 g of 15% T12 phareidin original drug A, add 6 times the volume (6 mL) of chloroform, reflux extraction at 80 ° C for 40 min, filter and concentrate under reduced...
Embodiment 2
[0285] (1) Preparation method of 15% T12 picrodermin original drug A
[0286] Other conditions are the same as in Example 1, except that water with twice the volume of the filtrate is used as a precipitant, and the effect is similar to that of Example 1.
[0287]
[0288] (2) Quality testing method of 15%T12 picratine original drug A
[0289] ①Preparation of characteristic extract-same as Example 1.
[0290] ②Feature extraction IGD carbon NMR fingerprint detection
[0291] With embodiment 1.
[0292] ③Fingerprint analysis of IGD carbon NMR spectra of feature extracts
[0293] 1) Identification
[0294] In the IGD carbon NMR fingerprint of the characteristic extract of 15% T12 pharethin original drug A, the characteristic signal of 4-OH-β-dihydrofuran sesquiterpene polyol esters is clearly displayed. According to the chemical shift of its parent nucleus signal and its C-15 characteristic peak signal, 12 4-OH-β-dihydroagarfuran sesquiterpene polyol ester compounds picroc...
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