A kind of determination method of strychnin biological sample
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A technology of strychnin, biological samples, applied in the field of medicine
Active Publication Date: 2017-05-31
LUNAN PHARMA GROUP CORPORATION
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[0005] At present, there are few reports on the detection methods of strychnin in vivo drug content
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Embodiment 1
[0027] Embodiment 1 Methodological investigation of the detection method of the present invention
[0028] 1. Preparation of standard solution
[0029] (1) Preparation of standard series solutions
[0030] Accurately weigh an appropriate amount of strychnin, place it in a 10mL measuring bottle, dissolve in 0.1% formic acid water and dilute to the mark to obtain a standard stock solution with a concentration of 1.0mg / L. Precisely measure an appropriate amount of standard stock solution, dilute it with 0.1% formic acid water gradient, and prepare concentrations of 80.0, 40.0, 8.00, 2.00, 0.400, 0.0800, 0.0400 μg·mL -1 standard series solutions.
[0031] (2) Preparation of internal standard solution
[0032] Accurately weigh an appropriate amount of Dinghuan Astragalol reference substance, place it in a 10mL measuring bottle, dissolve it in methanol and dilute to the mark to obtain a concentration of 1.0mg·mL -1 stock solution. Precisely measure 0.1mL of the stock solution, ...
Embodiment 2
[0057] Example 2 Preliminary Pharmacokinetic Test Method of Strychnin Solution in Rats
[0058] Take 8 SD rats with a body weight of about 300g and divide them into 2 groups, 4 rats in each group. One group is intravenously injected with strychnin solution at a dose of 20 mg / kg, and the other group is given strychnin solution by gavage , the dose is 20mg / kg. On the day of administration, the body weight was weighed, and the dosage and corresponding volume were accurately calculated according to the body weight. Rats in each group were given blank blood from the subclavian vein before administration. 0.2ml of blood was collected at 0.0167, 0.0833, 0.167, 0.333, 0.5, 0.75, 1, 1.5, 2, 3, and 4 hours after intravenous administration; , 0.2ml of blood was collected at 2, 3, and 4 hours. Immediately after the blood was taken out, it was mixed with an equal volume of 0.3% formic acid saline, centrifuged at 4000rpm for 10min, and the upper layer of clarified plasma was taken, and qu...
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Abstract
The invention relates to a method for determining loganin sapogenin in a biological sample and belongs to the technical field of medicine.The method includes that concentration of the loganin sapogenin in the biological sample is determined by ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry, wherein methyl alcohol in the biological sample serves a precipitation solvent; gradient elution is conducted, and a flow phase under a liquid phase condition consists of water with 0.1% formic acid and the methyl alcohol; cycloastragenol acts as an internal standard for determining the loganin sapogenin in the biological sample.The method for determining the loganin sapogenin in the biological sample has the advantage that the LC-MS-MS determining method satisfies the analysis requirements of Chinese Pharmacopoeia (2015 edition) and Technical Guidelines for Non-clinical Pharmacokinetic Studies on Chemical Drugs promulgated by SFDA (State Food and Drug Administration) in 2014 on biological samples in terms of accuracy, precision, specificity, stability, recovery rate, matrix effects and the like.
Description
technical field [0001] The invention belongs to the technical field of medicine and relates to a method for measuring a loganin biological sample. Background technique [0002] Strychnin is the saponin of strychnin, the main component of the commonly used Chinese medicinal material Cornus officinalis, with a relative molecular mass of 228, and its structural formula is as follows: [0003] [0004] Strychnin is the active ingredient of strychnin to play the role of immune regulation, anti-shock, anti-lipid peroxidation, etc. It has significant pharmacological effects, but also has relatively high toxicity, and the clinical treatment window is narrow. The development of strychnin requires a stable, reliable and precise detection method, which can detect the dynamic changes of trace amounts of strychnin in the organism after administration, and timely understand the absorption and metabolism of the drug. In the later stage of clinical medication, it is also necessary to mo...
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