Method for simultaneously detecting contents of six components in Sanwu capsule
A technology of black glue pills and content, which is applied in measurement devices, material separation, and analysis of materials, etc., can solve the problems of low accuracy, low content of diester alkaloids, and inability to quantify, so as to ensure quality stability, Good reproducibility and good resolution
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Embodiment 1
[0027] Example 1: Sanwu capsule sample pretreatment
[0028] Before the determination of HPLC content, the sample of Sanwu capsules to be tested is pretreated, that is, extracted. The purpose of extraction is twofold. One is to reduce the detected impurities in the preparation of Chinese patent medicines, and the other is to extract as much as possible of the components to be tested. It is separated from the pharmaceutical preparations to increase the peak area of the characteristic peaks and improve the accuracy. According to the prescription composition of Sanwujiao pills, we combine the solubility and other properties of the drug;
[0029] (1) Method 1: Weigh 1.5g of Sanwu capsule powder (passed through a 50-mesh sieve), add 5mL of petroleum ether, ultrasonicate at 25°C for 5min, let stand, evaporate the petroleum ether below 40°C; add 3mL of ammonia water to wet ;Add 20mL of ether, weigh it, and ultrasonically extract it at 25°C for 60 minutes, make up the loss with eth...
Embodiment 2
[0031] Embodiment 2: sample purification and detection
[0032] 1. Preparation of magnetic graphene-based adsorbent
[0033] (1) Weigh tris(2-aminoethyl)amine (0.5g) into a round bottom flask, add 100mL of methanol to dissolve, then add methyl acrylate (MA) (2.4g) into the round bottom flask at 30°C Add 2.0g of triethylenediamine after 24 hours of reaction at low temperature, and continue to react at 30°C for 24h. The reaction product is rotary evaporated at 30°C to obtain a crude product; the crude product is dissolved in methanol solution, and then 2.4g of methyl acrylate is added. After reacting at 30°C for 24 hours, 2.0 g of triethylenediamine was added, and the reaction was continued at 30°C for 24 hours to obtain polyamide polyamide dendrimers;
[0034] (2) Add 100mL ethylene glycol to a 250mL round bottom flask, and 2.0g FeCl 3 ·6H 2 O, 2.0g Ni(NO 3 ) 2 ·6H 2 O, 6.0g NaAc and 0.8g NaOH were added to ethylene glycol in sequence, ultrasonically dissolved until the s...
Embodiment 3
[0049] Example 3: Repeatability Verification
[0050] Take 6 parts of Sanwu capsule samples (batch number: 200903), each 1.5g, use method 1 to extract and use the method of embodiment 2 to purify, prepare 6 solutions of the test product to be tested, and use the conditions of step 3 of embodiment 2 to carry out For liquid phase detection, each sample was injected twice, and the peak areas of the 6 components in the 6 samples were measured at a detection wavelength of 245nm, and then substituted into the regression equation in step 4 of Example 2 to calculate the 6 components to be tested in 6 parallel experiments. The content of the components to be tested, the average content of the 6 components to be tested in Sanwujiao Pills (batch number: 200903) is as follows (per 1.5g): 8-deacetyl yunaconitine (0.65mg), aconitine (0.14mg ), benzoyl aconitine (0.51 mg), benzoyl aconitine (0.63 mg), benzoyl aconine (0.19 mg), emodin (0.02 mg); and calculate Measure the RSD of component co...
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