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Thiol medicine content detection method

A detection method, the technology of thiols, applied in the detection field, can solve the problems of complex operation steps, low detection sensitivity, high cost, etc., and achieve the effects of accurate measurement results, short analysis time, and easy operation

Inactive Publication Date: 2016-06-01
INST OF PROCESS ENG CHINESE ACAD OF SCI
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Problems solved by technology

Such as CN102520093A proposes a kind of method that ion chromatography tandem ultraviolet detection method measures Caputoli content, this method adopts ion chromatography cation exchange system and ultraviolet detector to be used in conjunction, according to the difference of retention behavior of substance on chromatographic column, select suitable separation conditions, and then select the optimal UV detection wavelength, it can separate and detect captopril with relatively high sensitivity. Early, can not be effectively separated; In addition, the chemical structure of thiol drugs generally lacks matching UV or fluorescence signal response, resulting in low sensitivity and poor reproducibility of the method
[0004] Existing literatures have used the method of derivatization pretreatment to detect thiol drugs, such as the literature has reported the use of 3-bromomethyl-isopropylantipyrine (BMP) as a derivatization reagent to shield the thiol group in the capitol structure group, can separate and detect captopri (3-Bromomethyl-propyphenazone as a new derivatization reagent for high performance liquid chromatography of captopriland hydrochlorothiazide with UV-detection, Biomed. Chromatogr., 1998, 12:57) under relatively high sensitivity, but this method derivation process needs to add potassium carbonate as a catalyst, operation The steps are relatively complicated and the cost is high; CN102977113A discloses a method for detecting thiols based on a coumarin chromene derivative, and the coumarin chromene derivative is 8,9-dihydro-2H-cyclopenta[ b]pyrano[2,3-f]chromene-2,10(7AH)-dione (abbreviation: CPC), the detection method is based on CPC, quantitatively detects the content of mercaptan in the HEPES solution whose pH is 7.4; CN103575727A discloses A kind of reagent that detects thiol, described reagent is maleimide derivative: 2-(2,5-dioxo-2,5-dihydro-1H-pyrrol-1-yl)-1H- Benzo[de]isoquinoline-1,3(2H)-dione; CN102183471A discloses a quantitative detection method and kit for mercaptans, said method and kit are based on a chromene derivative NPC:7 -nitro-2,3-dihydro-1H-cyclopenta[b]chromen-1-one, for quantitative detection of thiols in pH 7.0 buffer solution
However, these methods cannot avoid the polymerization of thiols and the detection sensitivity is not high

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Examples

Experimental program
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Effect test

Embodiment 1

[0053] To measure the amount of captopril in the solution:

[0054] (1) Adjust the pH of the captopril sample solution with a concentration of 35ppm to 7, add 45ppm reducing agent TCEP, stir rapidly for 5min, and the stirring intensity is 200r / min to obtain the reduced product;

[0055] (2) Add 2,6-dimethoxybenzoquinone as a quinone derivatization reagent to the reduction product, the dosage is 40ppm, react in a water bath at 30°C for 15min, and the derivatization product can be obtained. The sample is 0.45μm Standby after filtering through the filter head, the generation mechanism of the derivatized product is as follows: figure 1 shown;

[0056] (3) Separation and detection of derivatized products using high-performance liquid chromatography in series with ultraviolet detectors. The chromatographic column is an AgilentPH5-C18 column (100×2.1mm1.d, 2.7μm), the column temperature is 35°C, and the mobile phase is 80% Containing 0.1wt% phosphoric acid aqueous solution + 20% ac...

Embodiment 2

[0063] To measure the content of tiopronin in the solution:

[0064] (1) The pH of the tiopronin sample solution with a concentration of 45ppm is adjusted to 6, and 40ppm reducing agent sodium borohydride is added, and the stirring speed is 3min, and the stirring intensity is 150r / min to obtain the reduced product;

[0065] (2) Add 2-hydroxy-1,4-naphthoquinone to the reduction product as a quinone derivatization reagent, the dosage is 50ppm, and react in a water bath at 25°C for 10min to obtain the derivatization product. The sample is 0.45μm After the filter head is filtered, it is ready for use;

[0066] (3) Separation and detection of derivatized products using high-performance liquid chromatography in series with ultraviolet detectors. The chromatographic column is an AgilentPH5-C18 column (100×2.1mm1.d, 2.7μm), the column temperature is 30°C, and the mobile phase is 70% Containing 0.2wt% phosphoric acid aqueous solution + 30% acetonitrile, the flow rate is 0.5mL / min, the...

Embodiment 3

[0070] To measure the amount of mesna in a solution:

[0071] (1) Adjust the pH of the mesna sample solution with a concentration of 25ppm to 7.5, add 30ppm reducing agent tributylphosphine, stir rapidly for 4 minutes, and the stirring intensity is 175r / min to obtain the reduced product;

[0072] (2) Add 1,2-anthraquinone as a derivatizing agent to the reduced product, the dosage is 63ppm, and react in a water bath at 28°C for 18 minutes to obtain the derivatized product, and the sample is filtered through a 0.45 μm filter head for later use;

[0073] (3) The derivatized products were separated and detected by high-performance liquid chromatography with a series ultraviolet detector. The chromatographic column was an AgilentPH5-C18 column (100×2.1mm1.d, 2.7μm), the column temperature was 40°C, and the mobile phase was 60% Containing 0.1wt% phosphoric acid aqueous solution + 40% acetonitrile, the flow rate is 0.6mL / min, the injection volume is 30μL, and the detection wavelength...

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Abstract

The invention provides a thiol medicine content detection method. The thiol medicine content detection method includes the following steps that 1, a reducing reagent is added in a thiol medicine solution, and a dithio polymer in the solution is reduced to obtain a reduced product solution; 2, the reduced product solution and a quinones derivatization reagent perform derivatization reaction to obtain a derivatization product solution; 3, the content of a derivatization product is detected to obtain the content of a thiol medicine. According to the method, the thiol medicine is subjected to derivatization pretreatment by using a quinone compound after being reduced, the stable derivatization product is quickly generated, then the content of the derivatization product is separated and determined by adopting a detection means, and the thiol medicine content in a sample can be accurately calculated. The thiol medicine content detection method is high in recovery rate, simple and easy to operate, high in accuracy rate, quick to detect and high in sensitivity and can be used in the fields of detection of the thiol medicine content, study of human body fluid pharmacokinetics and the like.

Description

technical field [0001] The invention belongs to the technical field of detection, and relates to a quantitative detection method of thiol drugs, in particular to a method for separating and detecting thiol drugs by using derivatization pretreatment and liquid chromatography-ultraviolet detector. Background technique [0002] Thiol drugs are a general term for a class of drugs with a sulfhydryl structure, mainly including compounds such as mesna, captopril, cysteine ​​and tiopronin. It is widely used in the field of medicine for the treatment of diseases such as heart failure, X-ray damage, hepatitis and bloody cystitis. Many of these drugs have certain side effects, which may cause symptoms such as cough, headache, itching, and chest tightness. [0003] Common analytical and quantitative methods for thiols include liquid chromatography, ion chromatography, ultraviolet, electrochemical, evaporative light scattering, and near-infrared spectroscopy, as well as titration and op...

Claims

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Application Information

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IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 赵赫杜朋辉曹宏斌张笛刘晨明
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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