Detection method for limonins components in szechwan Chinaberry fruit extractive
A technology of limonoids and detection method, which is applied in the field of detection of limonoids in Toosendan extract, can solve problems such as not seen, and achieve the effects of strong specificity, easy implementation, and scientific methods
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Embodiment 1
[0020] The preparation of embodiment 1 toosendan extract
[0021] Take 4 kg of Toosendan medicinal material, crush it into coarse powder, reflux extract with 50 L of 75% ethanol for 3 times, each time for 2 hours, combine the extracts, recover the solvent under reduced pressure, and obtain 550 g of Toosendan extract, disperse it with 4 L of water, and disperse it with acetic acid The ethyl acetate was shaken and extracted 4 times, 4 L each time, the ethyl acetate extracts were combined, and the solvent was recovered under reduced pressure to obtain Toosendan extract (180 g).
Embodiment 2
[0022] The HPLC / ELSD detection method of limonoids component in the Toosendan extract of embodiment 2
[0023] (1) Preparation of reference substance solution: take 1-deacetyl-niporinin B (reference substance 1: 0.7746mg / ml), niporinin A (reference substance 2), and niporinin B (reference substance 3), toosendanin (reference substance 4) and toosendanin (reference substance 5; 0.3445mg / ml) appropriate amount, accurately weighed, and prepared with methanol, to obtain.
[0024] (2) Preparation of the test solution: take an appropriate amount of Toosendan medicinal material sample or reference medicinal material, grind it finely (through a No. 3 sieve), take about 5.0g, accurately weigh it, place it in a 100ml measuring bottle, and accurately add ethyl acetate 50ml of ester, plugged tightly, weighed, extracted under reflux for 3 hours, placed at room temperature, weighed, made up for lost weight with ethyl acetate, shaken well, filtered, took the subsequent filtrate, accurately m...
Embodiment 3
[0033] TLC identification of limonoids in Example 3 Toosendan extract
[0034] Toosendan medicinal material (MT-1), 5 batches of commercially available Toosendan medicinal herbal pieces (MTp-1~MTp-5) and Toosendan extract (MT-2) were taken respectively, and Toosendan as a control medicinal material (MT-R) and 1-deacetyl nipoorinine B reference substance (1) carry out TLC identification jointly (see attached figure 2 ). Reference substance solution, need testing solution are with embodiment 2.
[0035] Thin-layer chromatography identification: test according to thin-layer chromatography (Appendix VIB of Chinese Pharmacopoeia 2010 Edition), draw each 10-20 μ l of each reference substance solution and sample solution, respectively spot on the same silica gel G thin-layer plate, and use petroleum ether ( 60~90°C)-ethyl acetate (1:1) as the developer, develop, take out, dry in the air, spray with 10% sulfuric acid ethanol solution, and heat at 105°C until the chromatographic spo...
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