Detection method of traditional Chinese medicine preparation compound Chuanbeijing tablet
A detection method and a technology for comparing medicinal materials, which are applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of identifying ephedra root and Bai Wei, and achieve the same extraction effect, stable baseline of the map, and good separation
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preparation example Construction
[0058] Preparation of reference substance solution: take 10 mg of ephedrine hydrochloride reference substance, accurately weigh, put in a 100ml measuring bottle, add methanol to dilute to the mark, shake up, accurately measure 2ml, put in a 25ml measuring bottle, add mobile phase to dilute to the mark , Shake well to make a reference solution containing 8 μg of ephedrine hydrochloride per 1 ml.
[0059] Preparation of the test solution: Take 20 tablets of this product, grind them finely, accurately weigh 0.4-0.6g of this product, put it in a 100ml measuring bottle, add 50-70ml of methanol, and ultrasonicate for 15-20min at a power of 120W and a frequency of 59KHz , add methanol to dilute to the mark, shake well, filter, and discard the initial filtrate to obtain the test solution.
[0060] Determination method: Accurately draw 8-12 μl each of the reference substance solution and the test solution, inject it into a liquid chromatograph, and measure; each tablet of this product ...
Embodiment 1
[0069] (1) TLC qualitative identification
[0070] TLC qualitative identification of ephedrine and ephedrine A: take 10 tablets of this product, grind finely, add 30ml of water to dissolve, shake and extract twice with ether, the amount of ether used each time is 20ml; discard the ether solution , the water liquid is evaporated to dryness in a water bath, the residue is added with ethanol 20ml to dissolve, filtered, the filtrate is evaporated to dryness in a water bath, and the residue is added to 1ml of methanol to dissolve, as the test solution; Add methyl alcohol and make every 1ml containing the mixed solution of ephedrine reference substance and ephedrine A reference substance each 1mg, as reference substance solution; 10 μl each of the test solution and the reference solution were spotted on the same silica gel G thin-layer plate, and the toluene-methanol-ammonia mixture with a volume ratio of toluene:methanol:ammonia = 10:4:1 was used as the developer, and developed for...
Embodiment 2
[0081] (1) TLC qualitative identification
[0082] Qualitative identification of ephedrine and ephedrine A by TLC: take 10 tablets of this product, grind finely, add 40ml of water to dissolve, shake and extract with ether for 3 times, the amount of ether used each time is 30ml; discard the ether solution , the water liquid water bath evaporates to dryness, the residue adds ethanol 30ml and makes dissolving, filters, and the filtrate water bath evaporates to dryness, the residue adds methanol 2ml and makes dissolving, as need testing solution; Get ephedrine reference substance and ephedrine A reference substance in addition, Add methyl alcohol and make every 1ml containing the mixed solution of ephedrine reference substance and ephedrine A reference substance each 1mg, as reference substance solution; 12 μl each of the test solution and the reference solution were spotted on the same silica gel G thin-layer plate, and the toluene-methanol-ammonia water mixture with a volume rat...
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