Detection method of formic acid in cefamandole nafate

A cefamandole sodium and detection method technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the adverse effects of the chromatographic system, blockage of the chromatographic system and other problems, and achieve the inhibition of formic acid dissociation, good stability and accuracy and high-precision effects

Inactive Publication Date: 2016-02-03
GUANGXI KELUN PHARMA
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Problems solved by technology

[0007] In the prior art, there is also the report of using hydrogen phosphate buffer as the mobile phase to detect formic acid (as HPLC measures the content of formic acid in secnidazole, Lin Daoming, Fu Zhaoli, Liang Guodong, etc. HPLC measures the content of formic acid in secnidazole[ C]. / / Proceedings of the 6th Chinese Pharmaceutical Association Academic Annual Conference 2006. 2006.; Simultaneous Determination of 6 Organic Acid Contents in Feed Additives by High Performance Liquid Chromatography, Zhao Yan, Zhang Fengping, Yang Fashu, etc. High Performance Liquid Chromatography Simultaneous determination of 6 kinds of organic acids in feed additives by chromatography[J]. Chinese Journal of Cereals and Oils, 2015, 30(2): 127-130.; Determination of formic acid and acetic acid in urine by high performance liquid chromatography, Feng Bin, Shao Hua , Cheng Xuemei, etc. Determination of formic acid and acetic acid in urine by high performance liquid chromatography [J]. Chinese Journal of Health Inspection, 2006, 16 (2): 207-208), however, hydrogen phosphate is a large polar substance, and the ion However, HPLC experiments often use organic solvents with low polarity. When hydrogen phosphate is not washed thoroughly, once a high-concentration organic solvent is used in the next experiment, the residual hydrogen phosphate will crystallize because it cannot be dissolved in organic solvents. Precipitation can easily lead to problems such as blockage of the chromatographic system, which will have an adverse effect on the chromatographic system

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  • Detection method of formic acid in cefamandole nafate

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Experimental program
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Effect test

Embodiment 1

[0028] 1. Instruments used: Agilent 1260 high performance liquid chromatograph (Agilent), DADG4212B detector (Agilent).

[0029] 2. Chromatographic conditions:

[0030] Chromatographic column: ThermoHypersilGoldaQ4.6*250mm, 5μm;

[0031] Mobile phase: phosphoric acid aqueous solution with a volume concentration of 0.02%;

[0032] Detection wavelength: 210nm;

[0033] Flow rate: 1.0ml / min;

[0034] Column temperature: 30°C.

[0035] 3. Sample:

[0036] 3.1) Formic acid solution: (That is, take 0.1034g of formic acid (mass fraction is 93.38%) and add water to 100ml, then take 1ml from it and add water to 100ml).

[0037] 3.2) Cefamandole sodium solution: (i.e. get 1.0101g of cefamandole sodium finished product (manufactured by the applicant) and add water to be settled to 10ml).

[0038] 3.3) Place the cefamandole sodium solution described in 3.2) above in a water bath at 60° C. for 30 minutes and destroy it for 30 minutes, take it out and cool it, and obtain the destr...

Embodiment 2

[0047] Embodiment 2: the methodology validation of the method of the present invention

[0048] 1. Limit of detection, limit of quantitation, linearity experiment

[0049] Detection limit: 12.1ng

[0050] Quantitation limit: 43.56ng

[0051] Linear range: Weigh 0.1169g of formic acid test solution (mass fraction 93.38%), converted to 0.1090g of formic acid, dilute to 100ml with water, shake well as stock solution.

[0052]Pipette 0.2ml, 0.5ml, 1.0ml, 1.5ml, 1.8ml, 2.0ml of formic acid stock solution respectively, and set the volume to 10.0ml; inject 20ul of each sample for detection, take the formic acid concentration on the abscissa, and the corresponding peak area on the ordinate , to make a standard curve, such as Figure 6 shown.

[0053] Regression equation: Area=1.1433*Amt+2.2484

[0054] The correlation coefficient R^2=0.9994.

[0055] Experiments show that the linearity is good when the concentration of formic acid is in the range of 21.8 μg / ml to 218.0 μg / ml.

...

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Abstract

The invention discloses a detection method of formic acid in cefamandole nafate. According to the method, a liquid chromatography is used for detecting; and a mobile phase used in a detection process is a phosphoric acid water solution with the volume concentration of 0.02%-0.1%. By taking the phosphoric acid water solution with the volume concentration of 0.02%-0.1% as the mobile phase for detecting the formic acid in the cefamandole nafate in a liquid chromatography, the dissociation of the formic acid can be effectively inhibited, and retention time and separation degree of the formic acid can be improved very well, so that the separation degrees of the formic acid and front and back adjacent impurity peaks are 3.68 and 1.78 respectively; and the blocking of a chromatographic column is not caused. Furthermore, the method has high accuracy and precision and good stability, and is easy to realize in industrialization.

Description

technical field [0001] The invention relates to a detection method for formic acid, in particular to a detection method for formic acid in cefamandole sodium. Background technique [0002] Cefamandole sodium, also known as cefadoxazole; second-generation cephalosporin antibiotics. Cefamandole sodium enters the body and is rapidly hydrolyzed into cefamandole, which has a bactericidal effect. The mechanism of action is to bind to the penicillin-binding proteins (PBPs) on the bacterial cell membrane, acylate the transpeptidase, inhibit the synthesis of the bacterial septum and cell wall, affect the cross-linking of the mucopeptide components of the cell wall, and inhibit cell division and growth. The form becomes elongated and finally dissolves and dies. [0003] When cefamandole sodium is decomposed into free cefamandole, it will be accompanied by the production of formic acid. Formic acid belongs to the third category of reagents, and according to the ICHQ3c guidelines, th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 张立昭欧世强黎杏玉李永鑫罗丽柠吴琼谭佳万阳浴程志鹏葛均友刘思川
Owner GUANGXI KELUN PHARMA
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