High performance liquid chromatography-mass spectrometry detection method for nafil medical intermediates
A high-performance liquid chromatography and mass spectrometry detection technology, which is applied in the field of drug detection, can solve problems such as the absence of tetrahydrocarboline hydrochloride-related detection methods, and achieve rapid and accurate qualitative and quantitative analysis, super separation ability, and accurate and reliable detection results Effect
Inactive Publication Date: 2020-06-12
广西东盟食品检验检测中心
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[0004] The purpose of the present invention is to provide a high-performance liquid chromatography-mass spectrometry detection method for nafil pharmaceutical interme
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Embodiment 1
[0029] A high-performance liquid chromatography-mass spectrometry detection method for a nafil pharmaceutical intermediate, comprising the following steps:
[0030] (1) Solid sample preparation
[0031] Take an appropriate amount of solid sample, grind, pulverize and mix evenly, accurately weigh 1g of sample (accurate to 0.001g) into a 50mL volumetric flask, accurately add 40mL of methanol, ultrasonically extract for 15min, put it at room temperature, and dilute to the mark with methanol. Transfer to a 100mL centrifuge tube, centrifuge at 5000r / min for 5min, filter the supernatant with a 0.22μm organic phase filter, and dilute appropriately with 50% methanol aqueous solution to the linear range according to the actual concentration, and set aside.
[0032] (2) Preparation of oil-containing samples
[0033] Take an appropriate amount of the contents of the soft capsule sample and mix evenly, accurately weigh 1g (accurate to 0.001g) and place it in a 50mL volumetric flask, add ...
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The invention discloses a high performance liquid chromatography-mass spectrometry detection method for nafil medical intermediates, and belongs to the field of drug detection. The method comprises the following steps: measuring tetrahydrocarboline hydrochloride serving as a food and traditional Chinese medicine intermediate by using an ultra-high performance liquid chromatography-tandem mass spectrometry method, dissolving a sample by using a 50% methanol solution, performing ultrasonic extraction, performing detecting in an ESI source positive ion mode by using a liquid chromatography-tandemmass spectrometry method, performing collecting by using a multi-reaction monitoring (MRM) mode, and performing quantifying by using an external standard method. The method has the advantages of simple operation of detection steps, strong specificity, high sensitivity and an accurate and reliable detection result, and provides a more reliable confirmation basis for supervision of illegally addedchemicals in food and health food. Aiming at the fact that no related detection method of the medical intermediate tetrahydrocarboline hydrochloride exists in China at present, the blank of the compound analysis and detection method in China is filled.
Description
technical field [0001] The invention relates to the field of drug detection, in particular to a high-performance liquid chromatography-mass spectrometry detection method for a nafil pharmaceutical intermediate. Background technique [0002] At present, the State Food and Drug Administration has issued a number of supplementary inspection methods for commonly illegally added impotence drugs in food and health food. However, under the high-pressure attack, criminals are opportunistic and add other analogues outside the detection range of the current standard, such as cis-(1R,3R)-1,2,3,4-tetrahydro-1-(3,4- Methylenedioxyphenyl)-9H-pyrido[3,4-B]indole-3-carboxylic acid methyl ester hydrochloride (abbreviation: tetrahydrocarboline hydrochloride, chemical formula: C 20 h 19 ClN 2 o 4 , CAS No.: 171752-68-4), this substance is a new type of tadalafil derivative, which is the key intermediate for the synthesis of tadalafil, which has not yet been approved for marketing in my cou...
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Login to View More IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 农毅清戴向东韦环周嵩煜覃文霞王警刘珈伶
Owner 广西东盟食品检验检测中心