A kind of identification and content determination method of traditional Chinese medicine gel
A determination method and gel technology, which are applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of low content of target substances, abnormal spots, complex composition of crude extract, etc., and achieve the effect of reducing pollution and simple method.
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Embodiment 1
[0046] TLC identification method:
[0047] (a) Preparation of the test solution: take 3 g of Moschus trifloxacin gel and add 30 mL of 70% ethanol, seal it, soak it for 30 min, and ultrasonicate for 4 min; heat to reflux for 1.5 h, cool to room temperature, shake and extract 3 times with chloroform, 3 The chloroform used for this time was 30mL, 20mL and 20mL respectively, the filtrate was evaporated to dryness, the residue was dissolved in 1mL of absolute ethanol, and shaken well to obtain the product;
[0048] Preparation of control solution: take menthol reference substance and borneol reference substance plus absolute ethanol to make solutions containing 5mg and 10mg in each 1mL;
[0049] Thin-layer chromatography experiment: Take 5 μL of the test solution and the reference solution, respectively, and spot on the same silica gel G thin-layer plate, use benzene-ethyl acetate (18:2) as the developing agent, develop, and the span is 13cm. Take it out, dry it in the air, spray ...
Embodiment 2
[0055] TLC identification method:
[0056] (a) Preparation of the test solution: Take 4 g of Moschus trifloxacin gel plus 50 mL of 70% ethanol, seal it, soak for 30 min, and ultrasonic for 3 min; heat to reflux for 1 h, cool to room temperature, shake and extract with chloroform 3 times, 3 times The chloroform used was 30mL, 20mL and 20mL respectively, the filtrate was evaporated to dryness, the residue was dissolved in 1mL of absolute ethanol, and shaken well to obtain the product;
[0057] Preparation of control solution: take menthol reference substance and borneol reference substance plus absolute ethanol to make solutions containing 5mg and 10mg in each 1mL;
[0058] Thin-layer chromatography experiment: draw 5 μL of the test solution and the reference solution, respectively, and spot on the same silica gel G thin-layer plate, use benzene-ethyl acetate (18:2) as the developing agent, develop, and the span is 14cm. Take it out, dry it in the air, spray it with 2% vanillin...
Embodiment 3
[0073] Determination of camphor, borneol and menthol content by headspace gas chromatography:
[0074] 1.1 Chromatographic conditions: DB-WAX quartz capillary column (30m×0.320mm×0.5μm); carrier gas is high-purity nitrogen, flow rate 1.5mL / min; hydrogen flame ionization detector; temperature program, initial temperature 130°C, Keep for 6 minutes, rise to 180°C at 12°C / min and hold for 4 minutes; split ratio 25:1; inlet temperature: 250°C; detector temperature: 260°C.
[0075] 1.2 Preparation of the test solution:
[0076] A. Take 3g of Shuhuoling gel, add 30mL of methanol, seal it, and soak it for 20min;
[0077] B. Reflux for 1 hour, cool to room temperature, and take the filtrate after passing through a 0.22 μm filter membrane;
[0078] C. Take a solid-phase extraction column, activate it with water, pass the filtrate in B through the column, elute with chloroform, evaporate the eluent to dryness, add methanol to the residue to make up to 10 mL, shake well, and obtain.
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