Detection method for the active ingredients of Xiaoer Jianwei Syrup
A detection method and a technology of active ingredients, applied in the field of medicine, can solve the problems of inability to fully monitor the quality of medicines, and achieve the effects of moderate Rf value, simple preparation method, and clear map
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Embodiment 1
[0076] Example 1 Identification item
[0077] Instruments and Reagents
[0078] DigiStore 3 digital imaging system (CAMAG, Switzerland); double-slot expansion cylinder (Shanghai Xinyi Instrument Factory);
[0079] Silica gel G prefabricated plate (Qingdao Ocean Chemical Factory), silica gel G prefabricated plate (Taizhou Luqiao Sijia Biochemical Plastic Factory, Taizhou City, Zhejiang Province); TLC Silica 60 (Merck ordinary silica gel G plate); self-made plate (with 0.3% carboxymethyl cellulose) Silica gel G plate (thickness: 500 μm) with sodium as binder; self-made plate (silica gel G plate containing 1% sodium hydroxide).
[0080] Chemical reagents: cyclohexane, ethyl acetate, methanol, glacial acetic acid, 95% ethanol, sodium hydroxide, all of which are of analytical grade.
[0081] Reference substance and reference medicinal material: lotus leaf reference medicinal material (batch number: 121008-200505); tangerine peel reference medicinal material (batch number: 120904-...
Embodiment 2
[0091] Example 2 [Determination of Content] Content Determination of Paeoniflorin and Hesperidin
[0092] 1 Instruments and reagents
[0093] High performance liquid chromatograph: Agilent 1200.
[0094] Acetonitrile is of chromatographic grade, water is purified water, and other reagents are of analytical grade.
[0095] Paeoniflorin reference substance (batch number is 110736-201135, content is 96.5%; 110736-201136 content is 96.0%; 110736-201842 content is 97.4%;), hesperidin reference substance (batch number is 110721-201818, content 96.2%), the above are all provided by China National Institute for Food and Drug Control. Children's Jianwei Syrup samples and negative samples were provided by Guangzhou Wanglaoji Pharmaceutical Co., Ltd.
[0096] 2 Chromatographic conditions
[0097] Column: Welch ultimate XB-C18 (4.6×250mm, 5μm)
[0098] Kromasil 100-5 C18 (4.6×250mm, 5μm)
[0099] Capcell Pak MG S5 C18 (4.6×250mm, 5μm)
[0100] Mobile phase: Acetonitrile (A)-0.1% ph...
Embodiment 3
[0110] Example 3 Methodological validation
[0111] 5.1 Preparation of each solution
[0112] Preparation of reference solution: Precisely weigh the reference substances of paeoniflorin and hesperidin and place them in measuring bottles respectively, add appropriate amount of methanol to dissolve and dilute to the mark, and obtain the reference substance stock solution of paeoniflorin (about 0.25mg / ml) and orange. Pedroside reference stock solution (approximately 0.4 mg / ml).
[0113] Precisely draw the above two reference substance stock solutions, add methanol to dilute and dilute to volume, and prepare paeoniflorin reference substance solution (about 50 μg / ml) and hesperidin reference substance solution (about 30 μg / ml).
[0114] Preparation of the test solution: Precisely draw 5ml of this product into a 10ml volumetric flask, dilute to the mark with methanol, shake well, centrifuge, take the supernatant, filter it through a 0.45um microporous membrane, and take the subsequ...
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