Method for detecting pharmaceutical preparation for treating xiaoke disease
A technology of pharmaceutical preparations and detection methods, applied in the field of detection of pharmaceutical preparations, can solve the problems of single detection index, unfavorable drug quality, effective control, etc.
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Embodiment 1
[0063] The preparation of embodiment 1 capsule
[0064] [Prescription] Silkworm excrement 7.15kg and licorice 137.5g.
[0065] [Preparation method] For the above two flavors, take silkworm excrement and add 4 times the amount of 60% ethanol, soak overnight, slowly heat to boiling, reflux twice, each time for 1 hour, filter, combine the filtrates, recover ethanol, concentrate to a relative density of 1.01-1.06 (55°C), add 1 times the amount of water and continue to heat until boiling, cool, let stand overnight, take the supernatant, concentrate to a thick paste with a relative density of 1.06-1.15 (measured at 55°C), and set aside. Another licorice was decocted twice with 10 times the amount of water, each time for 2 hours, the filtrate was combined, left overnight to allow precipitation, the supernatant was concentrated to a thick paste with a relative density of 1.04-1.15 (measured at 55°C), and set aside. Combine the two thick pastes, add conventional auxiliary materials ac...
Embodiment 2
[0066] Embodiment 2HPLC method is measured the content of 1-deoxynojirimycin
[0067] 1 Instruments and reagents
[0068] Agilent-1200 high performance liquid chromatography includes: vacuum degasser, quaternary gradient pump, autosampler, diode array detector (DAD), Agilent-Chemistation data processing system (Agilent company); ultrapure water device (MilliQ-Gradient type); ultrasonic generator (Kunshan KQ-300E type).
[0069] 1-deoxynojirimycin reference substance (purchased from SIGMA Company), fluorenylmethoxycarbonyl chloride (purchased from SIGMA Company), acetonitrile was chromatographically pure, water was ultrapure water, and the rest of the reagents were analytically pure.
[0070] 2 Methods and results
[0071] 2.1 Preparation of reference substance solution, test solution and 1-deoxynojirimycin negative sample solution
[0072] 2.1.1 Preparation of reference solution
[0073] Take about 10 mg of 1-deoxynojirimycin reference substance, weigh it accurately, put i...
Embodiment 3
[0141] Embodiment 3HPLC method measures the content of 1-deoxynojirimycin
[0142] Accurately weigh 5 mg of 1-deoxynojirimycin reference substance, dilute with water to make a reference substance stock solution containing 0.1 mg per mL; accurately measure 1 mL of the reference substance stock solution, and accurately add NaHCO with a mass concentration of 1%. 3 Solution 1mL and 1mg / mL fluorenylmethoxycarbonyl chloride acetonitrile solution 1mL, mix well and carry out water bath reaction at 30°C for 20min, then dilute to 20mL with 30% acetonitrile as the reference solution.
[0143] Get the contents of the capsule prepared in Example 1 and grind finely, and accurately weigh 0.5g, add 30mL of water adjusted to pH 3 with concentrated hydrochloric acid, stir evenly, ultrasonically treat for 20min, and centrifuge to get the supernatant; Add an appropriate amount of water with a pH value of 3 to wash, centrifuge to combine the supernatant, and concentrate to 10mL; put the concentrat...
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