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Method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium

A technology of mercaptobenzothiazole and ceftriaxone sodium, which is applied in the detection field of 2-mercaptobenzothiazole, can solve the problems of inappropriate detection of 2-mercaptobenzothiazole and complicated detection methods, and achieves high sensitivity and durability. Good, good detection specificity

Active Publication Date: 2020-05-29
SICHUAN KELUN PHARMA RES INST CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Yang Weifeng et al. ("Identification of 2-Mercaptobenzothiazole Added in Counterfeit Drugs", "Drug Identification", 2010, Vol. 19, No. 13) studied the use of liquid chromatography-tandem quadrupole mass spectrometry To identify the 2-mercaptobenzothiazole added in the counterfeit medicine, however, the detection method recorded in the literature is too complicated, and the detection method is only suitable for qualitatively identifying whether the counterfeit medicine contains 2-mercaptobenzothiazole, so it is not Suitable for the detection of 2-mercaptobenzothiazole in the preparation process of ceftriaxone sodium

Method used

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  • Method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium
  • Method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium
  • Method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] S1. Preparation of solution:

[0042] 1. Prepare a blank solution: 50% acetonitrile in water;

[0043] 2. Preparation of the test solution: Weigh about 0.7 g of the test product of ceftriaxone sodium (Qilu Anti-Pharmaceutical Co., Ltd., the same below) and put it in a 10ml measuring bottle, add 50% acetonitrile water to dissolve and dilute to the mark, and mix well to get final product ;

[0044] 3. Prepare the impurity G reference substance solution: (1) First prepare the impurity G reference substance stock solution: accurately weigh about 1 mg of the impurity G reference substance, put it in a 25ml measuring bottle, add 50% acetonitrile to dilute to the mark, shake well, and use it as the impurity G reference substance stock solution; (2) prepare impurity G reference substance solution again: accurately measure (1) impurity G reference substance stock solution 0.9ml, put in 100ml measuring bottle, dilute to scale with 50% acetonitrile water, shake up, As impurity G...

Embodiment 2

[0054] The specificity experiment of embodiment 2 detection method

[0055] S1. Preparation of solution:

[0056] 1. Prepare a blank solution: 50% acetonitrile in water;

[0057] 2. Preparation of the test solution: Weigh about 0.7 g of the test product of ceftriaxone sodium, put it in a 10ml measuring bottle, add 50% acetonitrile water to dissolve and dilute to the mark, and mix well to obtain;

[0058] 3. Prepare impurity mixed reference substance solution: (1) first impurity mixed reference substance stock solution: weigh about 1.2 mg each of impurities A and C and place in a 10ml measuring bottle, weigh about 1.2 mg each of impurities B, E, F and H and place in 50ml measuring bottle, add 50% acetonitrile water to dissolve, dilute to the mark, and mix well to obtain the impurity mixed reference substance stock solution; (2) prepare the impurity mixed reference substance solution: accurately measure (1) impurity mixed reference substance stock solution 1ml Put in a 10ml me...

Embodiment 3

[0067] The linear methodology experiment of embodiment 3 detection method

[0068] S1. Preparation of solution:

[0069] Precisely weigh about 1 mg of the impurity G reference substance and put it in a 5ml measuring bottle, add 50% acetonitrile water to dissolve and dilute to constant volume, and then use it as the impurity G linear stock solution L 0 , and serially diluted to different concentrations as a series of linear solutions.

[0070] The linear solution preparation process is shown in the following table 1

[0071]

[0072]

[0073] S2. Chromatographic conditions:

[0074] Same as Example 1

[0075] S3. Chromatographic detection:

[0076] Take L in step S1 respectively 1 ~ L 9 , detected according to the chromatographic conditions in S2. Record the chromatogram.

[0077] result

[0078] With the concentration as the abscissa (X) and the peak area as the ordinate (Y), a linear regression analysis was performed. Calculate the square of the correlation co...

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Abstract

The invention relates to a method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium by using high performance liquid chromatography. The detection method adopts the following chromatographic conditions: a mobile phase A: a mixed solution of a phosphate buffer solution with the pH value of 6.05-6.45 and methanol; and a mobile phase B: an acetonitrile aqueous solution; wherein themobile phase A and the mobile phase B are used for gradient elution. The method is good in detection specificity, good in linear fitting, low in detection limit, high in sensitivity, good in quantification limit repeatability and good in durability.

Description

technical field [0001] The invention relates to a detection method for 2-mercaptobenzothiazole, in particular to a method for detecting impurity 2-mercaptobenzothiazole in ceftriaxone sodium by using high performance liquid chromatography. Background technique [0002] 2-Mercaptobenzothiazole is a common general-purpose vulcanization accelerator widely used in the rubber industry. Currently, 2-Mercaptobenzothiazole belongs to category 2A in the preliminary list of carcinogens released by the International Agency for Research on Cancer of the World Health Organization. carcinogen. Its structural formula is: [0003] [0004] Ceftriaxone sodium is the third-generation cephalosporin with broad-spectrum antibacterial activity developed by Roche Company in Switzerland, which is used for various infectious diseases caused by sensitive pathogenic bacteria. 2-Mercaptobenzothiazole is a by-product impurity that may be produced during the preparation of ceftriaxone sodium raw mat...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 王静于坤茹王利春王晶翼
Owner SICHUAN KELUN PHARMA RES INST CO LTD
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