Method for detecting drug concentration of minocycline in saliva sample
A technology for the concentration of minocycline and drugs, which is applied in the field of biological sample detection, can solve problems such as metal interference, and achieve the effect of improving detection sensitivity and reducing matrix effects.
Active Publication Date: 2021-03-09
国科卓越(北京)医药科技研究有限公司
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Problems solved by technology
[0004] The purpose of the present invention is to solve the problems of sample collection and metal interference in the matrix in the method of detecting the drug concentration of minocycline in animal saliva, establish a fast, sensitive and easy-to-operate method, and apply the verified method to domestic Saliva Pharmacokinetics of Minocycline in Rabbits
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Embodiment 1
[0021] Example 1: Study on Salivary Kinetics of Rabbits After Administration of Minocycline
[0022] It mainly includes the following steps:
[0023] S1, preparation of minocycline stock solution:
[0024] Accurately weigh minocycline, prepare an internal standard stock solution with methanol at a concentration of 1 mg / mL, the standard minocycline is batch number IF1800730A, with a purity of 89.9%, provided by Guangdong Liwei Pharmaceutical Co., Ltd.;
[0025] Prepare internal standard solution:
[0026] Accurately weigh the internal standard seven deuterated minocycline, use methanol to prepare the internal standard stock solution with a concentration of 1mg / mL, accurately measure the stock solution, and gradually dilute it with methanol to form an internal standard solution with a concentration of 1000ng / mL for subsequent use; the internal standard Heptadeuterated minocycline is batch number 36936, with a purity of 95%, provided by Guangdong Puen Scientific Instrument Co.,...
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The invention discloses a method for detecting the drug concentration of minocycline in a saliva sample. The method comprises the following steps of: collecting animal oral saliva samples at multipletime points before and after administration by using filter paper, measuring the saliva sampling weight by using a weight reduction method, drying the samples, and storing the samples at -20 DEG C forlater treatment; adding a saturated EDTAK2 solution and a precipitant (prepared from methyl alcohol and acetonitrile according to the volume ratio of 1: 1) into the filter paper, carrying out ultrasonic extraction for 10 min, carrying out vortex for about 30 s, carrying out centrifugation for 10 min, and taking supernatant for LCMS / MS analysis; establishing a standard curve for detecting minocycline in saliva; and quantitatively detecting the content of minocycline in the filter paper. The filter paper is used for adsorbing saliva, and the EDTAK2 solution is used for eliminating metal interference of the filter paper, so that the purpose of reducing the matrix effect is achieved. The detection method has the advantages of accurate and reliable verification result display, high recovery rate, and determination of the drug content in the animal saliva sample after drug administration.
Description
technical field [0001] The invention relates to the technical field of detection of biological samples, in particular to a method for detecting the drug concentration of minocycline in saliva samples. Background technique [0002] Minocycline hydrochloride, also known as minocycline hydrochloride, is a broad-spectrum antibacterial tetracycline antibiotic that can be used to treat periodontitis. This study intends to establish a rapid, sensitive, and easy-to-operate method for detecting the drug concentration of minocycline in rabbit saliva, in order to study the kinetics of the drug in saliva, formulate the time interval of administration and guide the development of pharmaceutical preparations. [0003] The main obstacles that need to be overcome in the development of detection methods for minocycline concentration in saliva are 1) it is difficult to collect saliva samples quantitatively; 2) minocycline is easy to complex with metal ions, which affects the quantification; 3...
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IPC IPC(8): G01N30/02G01N30/14
CPCG01N30/02G01N30/14G01N2030/045
Inventor 李敬来彭俊张天宏
Owner 国科卓越(北京)医药科技研究有限公司