Tripterygium wilfordii medicinal material and method for determining wilforlidea in tripterygium wilfordii polyglycosides tablet
A technology of triptolide A and its determination method, which is applied in the direction of measuring devices, material separation, and analysis materials, etc., to achieve the effects of reduced separation cost, good reproducibility, and good separation effect
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Embodiment 1
[0034] 1. Instruments and reagents
[0035] 1.1 Instrument: Shanghai Wufeng LC100 liquid chromatograph; TBE-200V high-speed countercurrent distribution chromatography;
[0036] 1.2 Reagents and reagents: standard triptolide A (source: Chengdu Master Biotechnology Co., Ltd.) phosphoric acid is analytically pure; acetonitrile is chromatographically pure; n-hexane is analytical grade; ethyl acetate is analytical grade; ethanol is analytical grade Grade; water is double-distilled water; chromatographic column is phenomenonex SYNERGI (250×4.6mm 4u); see Table 5 and Table 7 below for the source and origin of samples.
[0037] 2. Methods and results:
[0038] 2.1 Preparation of the reference substance solution of triptolide A: accurately weigh an appropriate amount of the reference substance of triptolide A, dissolve it with ethanol and dilute it into a reference solution containing 0.1 mg / mL of triptolide A;
[0039] 2.2 Preparation of the test solution:
[0040] ① Preparation of...
Embodiment 2
[0065] Preparation of triptolide A reference substance solution: accurately weigh an appropriate amount of triptolide A reference substance, dissolve it with ethanol and dilute it into a reference substance solution containing 0.1 mg / mL of triptolide A;
[0066] The preparation of need testing solution: 1. the preparation of solvent system: n-hexane, ethyl acetate, ethanol, aqueous solution are mixed by volume ratio 7:3:7:3, shake vigorously 5min then, be placed in separating funnel, static After layering, the upper phase solution was used as the stationary phase, and the lower phase solution was used as the mobile phase, and ultrasonic degassed for 15 minutes;
[0067] ② Rough extraction of samples: Take 20 tripterygium glycosides tablets and grind them finely (sample 3), accurately weigh 1.5g, add 50mL ethyl acetate, ultrasonicate for 30min, wash with 90mL ethyl acetate for 3 times, combine the filtrate and The washing solution was evaporated to dryness, and the residue was ...
Embodiment 3
[0075] Three kinds of Tripterygium wilfordii medicinal materials from different origins were taken to determine the content of triptolide A. The sample numbers and origins are shown in Table 6. Sample 7 was taken as an example:
[0076] Preparation of triptolide A reference substance solution: accurately weigh an appropriate amount of triptolide A reference substance, dissolve it with ethanol and dilute it into a reference substance solution containing 0.1 mg / mL of triptolide A;
[0077] The preparation of need testing solution: 1. the preparation of solvent system: normal hexane, ethyl acetate, ethanol, aqueous solution are mixed by volume ratio 3:2:3:2, shake vigorously then 5min, be placed in separating funnel, static After layering, the upper phase solution was used as the stationary phase, and the lower phase solution was used as the mobile phase, and ultrasonic degassed for 15 minutes;
[0078] ②Coarse extraction of samples: crush the medicinal material of Tripterygium w...
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