Detection method for compounded Sichuan fritillary bulb extract tablets
A technology of compound Chuanbei essence tablet and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of identification of unephedra root and Bai Wei, etc., and achieve equivalent extraction effect, stable baseline of the spectrum, and good separation Effect
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preparation example Construction
[0060] 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.
[0061] 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.
[0062] 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
[0071] (1) traits
[0072] This product is a sugar-coated tablet, yellowish brown after removing the sugar coating; fragrant and bitter.
[0073] (2) Microscopic observation
[0074] Take this product and observe it under a microscope. Calcium oxalate needle crystals form bundles, 32-144 μm long, present in mucus cells or scattered; Character-like or horseshoe-shaped, layered pattern can be seen.
[0075] (3) TLC qualitative identification
[0076] 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 eve...
Embodiment 2
[0086] (1) traits
[0087] This product is a sugar-coated tablet, yellowish brown after removing the sugar coating; fragrant and bitter.
[0088] (2) Microscopic observation
[0089] Take this product and observe it under a microscope. Calcium oxalate needle crystals form bundles, 32-144 μm long, present in mucus cells or scattered; Character-like or horseshoe-shaped, layered pattern can be seen.
[0090] (3) TLC qualitative identification
[0091] 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...
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