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Cefradine high performance liquid chromatography analysis method

A high-performance liquid phase analysis and cefradine technology, which is applied in the quality control field of cefradine, can solve the problems of unfavorable quantitative and qualitative detection of impurities, unfavorable separation of tetramethylguanidine, serious spectral peak tailing factor, etc., and achieves the realization of impurity quality control. And the effect of quality analysis of APIs

Active Publication Date: 2021-06-22
GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010]1) The chromatographic column and elution conditions of this method are not conducive to the separation of tetramethylguanidine, a new concern impurity in cephradine related substance I, and its peak tailing factor is serious , can not achieve better quality control of raw material impurities
[0011]2) The chromatographic conditions of this method cannot meet the baseline separation of 11 different impurities in the related substance I at the same time, which is not conducive to the quantitative and qualitative detection of impurities, not applicable Detection of Related Substance Ⅰ in Cephradine
[0012] The cephradine analytical method disclosed in the prior art mostly uses water / methanol: ammonium acetate as mobile phase elution system, adopts the chromatographic column of different fillers or detects by gas chromatography etc. This type of analysis method usually cannot meet the baseline separation effect of 11 different impurities in cephradine-related substance Ⅰ, nor can it achieve qualitative and quantitative detection of the new concern impurity tetramethylguanidine

Method used

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  • Cefradine high performance liquid chromatography analysis method
  • Cefradine high performance liquid chromatography analysis method
  • Cefradine high performance liquid chromatography analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] mobile phase:

[0063] Phase A: Phosphate buffer

[0064] Phase B: Methanol

[0065] Column: ACEC 18 -PFP(C 18 Bonded pentafluorophenyl silica gel packing)

[0066] Column temperature: 30°C

[0067] Injection volume: 25μL

[0068] Detection wavelength: 220nm

[0069] Flow rate: 1.0ml / min

[0070] Described a kind of high performance liquid phase analysis method of cephradine, comprises the following steps:

[0071] 1) Solution preparation

[0072] The preparation method of the mobile phase A is to take 2.72g of potassium dihydrogen phosphate, add water to dissolve and dilute to 1000mL, and adjust the pH to 3.0 with dilute phosphoric acid; the preparation method of the dilute phosphoric acid is to measure 69mL of phosphoric acid and dilute with water to 1000mL, shake well.

[0073] Accurately take by weighing an appropriate amount of this product, add mobile phase A to dissolve and quantitatively dilute to make a solution containing cephradine 6mg per 1ml, shak...

Embodiment 2

[0079] mobile phase:

[0080] Phase A: Phosphate buffer

[0081] Phase B: Methanol

[0082] Chromatographic column: ACE C 18 -PFP(C 18 Bonded pentafluorophenyl silica gel packing)

[0083] Column temperature: 30°C

[0084] Injection volume: 25μL

[0085] Detection wavelength: 220nm

[0086] Flow rate: 1.0ml / min

[0087] Described cephradine quality control method, comprises the following steps

[0088] 1) Solution preparation

[0089] Solution preparation method, with reference to embodiment 1

[0090] 2) Sample injection

[0091] 3) Elute with the linear gradient method, and the gradient settings are as follows:

[0092] stage V A相 :V B相

[0093] The resulting HPLC spectrogram is as figure 2 As shown, it can be seen that a total of 11 impurities were detected, and the peak shape of the impurities was good, and the monitoring of the new attention impurity tetramethylguanidine (t=15.188) was added. The peak order of each impurity was impurity A, dihy...

Embodiment 3

[0095] mobile phase:

[0096] Phase A: phosphate buffered saline,

[0097] Phase B: Methanol

[0098] Chromatographic column: ACE C 18 -PFP(C 18 Bonded pentafluorophenyl silica gel packing)

[0099] Column temperature: 30°C

[0100] Injection volume: 25μL

[0101] Detection wavelength: 220nm

[0102] Flow rate: 1.0ml / min

[0103] Described cephradine quality control method, comprises the following steps

[0104] 1) Solution preparation

[0105] Solution preparation method, with reference to embodiment 1

[0106] 2) Sample injection

[0107] 3) Elute with the linear gradient method, and the gradient settings are as follows:

[0108] stage V A相 :V B相

[0109] The resulting HPLC spectrogram is as image 3 As shown, it can be concluded that a total of 11 impurities were detected, and the peak shape of the impurities was good. On the basis of the detection of other impurities, the separation of the new concern impurity tetramethylguanidine (t=13.273) was ...

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Abstract

The invention discloses a cefradine high performance liquid chromatography analysis method, which adopts a phosphate buffer solution and methanol as mobile phases, adopts a special bonding C18 chromatographic column, can realize quality control of 11 impurities in cefradine, increases qualitative and quantitative analysis of a new concerned impurity tetramethylguanidine, and is favorable for realizing better quality control of the impurities of a bulk drug.

Description

technical field [0001] The invention belongs to the field of drug analysis, in particular to a quality control method for cephradine. Background technique [0002] Cephradine chemical name: (6R,7R)-7-[(R)-2-amino-2-(1,4-cyclohexadien-1-yl)acetamido]-3-methyl-8-oxo -5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylic acid, molecular formula: C 16 h 19 N 3 o 4 S molecular weight: 349.40. The structural formula is: [0003] [0004] Cefradine is a β-lactam antibiotic, used for acute pharyngitis, tonsillitis, otitis media, bronchitis and pneumonia and other respiratory tract infections, urogenital tract infections and skin and soft tissue infections caused by sensitive bacteria. In order to ensure the quality and efficacy of cephradine, it is necessary to control and detect related substances. [0005] At present, ChP, USP, BP and other national pharmacopoeias have included detection methods for cephradine-related substances, as follows: [0006] According to the Europea...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/86
CPCG01N30/02G01N30/06G01N30/34G01N30/36G01N30/74G01N30/8679
Inventor 李勇顾云孙金鑫林艾瑜程志伟
Owner GUANGDONG HUANAN PHARMACEUTICAL GROUP CO LTD