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Method for separating and measuring tebipenem pivoxil related substances

A technology of tibipenem ester and related substances, which is applied in the field of pharmaceutical analysis, can solve the problems of being inseparable from solvent peaks, difficult to separate, unable to effectively and accurately control related substances, etc., and achieve good separation and good peak shape

Inactive Publication Date: 2013-11-27
深圳万乐药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to strictly control the quality of drugs and ensure the safety and effectiveness of clinical medication, it is necessary to establish an inspection method for related substances of tibipenem, and the number of related substances of tibipenem is relatively large, and the impurity F is closely related to the main body of tibipenem. Similar properties, in general octadecyl silane bonded silica gel as filler column has the same chromatographic behavior with tibipenem and it is difficult to separate, and impurity A is a very polar substance, in general Octadecylsilane bonded silica gel is basically not retained on the chromatographic column of filler, and there is the situation that cannot be separated from the solvent peak, the existence of these problems makes the chromatographic peak of each related substance be separated by high performance liquid chromatography analysis method Separation is difficult, so it is impossible to effectively and accurately control the related substances that may exist in the sample

Method used

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  • Method for separating and measuring tebipenem pivoxil related substances
  • Method for separating and measuring tebipenem pivoxil related substances
  • Method for separating and measuring tebipenem pivoxil related substances

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1 Separation test

[0038] Instruments and reagents:

[0039] Instruments: Waters2695 high performance liquid chromatography, chromatographic grade acetonitrile (Merck), potassium dihydrogen phosphate (analytical grade).

[0040] Reagent: Tibipenem Reference Substance, Impurity A, B, C, D, E, F Reference Substance

[0041] Chromatographic conditions:

[0042] Chromatographic column: Ultimate AQ5μl250mm×4.6mm (Yuexu Technology Co., Ltd.)

[0043] Detector and detection wavelength: UV-220nm

[0044] mobile phase:

[0045] A: 0.025mol / L potassium dihydrogen phosphate solution (pH6.0)

[0046] B: Acetonitrile

[0047] Linear elution gradient:

[0048] time (min)

A％

B％

0

98

2

20

50

50

50

50

50

50.1

98

2

60

98

2

[0049] Flow rate: 1.0ml / min, injection volume: 10μl

[0050] Column temperature: 40°C

[0051] Solution preparation:

[0052] Control solution Ac...

Embodiment 2

[0059] The mensuration of embodiment 2 tibipenem ester crude drug

[0060] Instruments and reagents:

[0061] Instruments: Waters2695 high performance liquid chromatography, chromatographic grade acetonitrile (Merck), potassium dihydrogen phosphate (analytical grade).

[0062] Reagent: tibipenem raw material 20120627 (Shenzhen Wanle Pharmaceutical Co., Ltd.)

[0063] Chromatographic conditions:

[0064] Chromatographic column: Ultimate AQ5μl250mm×4.6mm (Yuexu Technology Co., Ltd.)

[0065] Detector and detection wavelength: UV-220nm

[0066] mobile phase:

[0067] A: 0.025mol / L potassium dihydrogen phosphate solution (pH6.0)

[0068] B: Acetonitrile

[0069] Linear elution gradient:

[0070] time (min)

A％

B％

0

98

2

20

50

50

50

50

50

50.1

98

2

60

98

2

[0071] Flow rate: 1.0ml / min, injection volume: 10μl

[0072] Column temperature: 40°C

[0073] Preparation of sample so...

Embodiment 3

[0075] The mensuration of embodiment 3 tibipenem granules

[0076] Instruments and reagents:

[0077] Instruments: Waters2695 high performance liquid chromatography, chromatographic grade acetonitrile (Merck), potassium dihydrogen phosphate (analytical grade).

[0078] Reagent: tibipenem granule 120801 (Shenzhen Wanle Pharmaceutical Co., Ltd.)

[0079] Chromatographic conditions:

[0080] Chromatographic column: Ultimate AQ5μl250mm×4.6mm (Yuexu Technology Co., Ltd.)

[0081] Detector and detection wavelength: UV-220nm

[0082] mobile phase:

[0083] A: 0.025mol / L potassium dihydrogen phosphate solution (pH6.0)

[0084] B: Acetonitrile

[0085] Linear elution gradient:

[0086] time (min)

A％

B％

0

98

2

20

50

50

50

50

50

50.1

98

2

60

98

2

[0087] Flow rate: 1.0ml / min, injection volume: 10μl

[0088] Column temperature: 40°C

[0089] Preparation of sample solution: Accurat...

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Abstract

The invention provides a method for separating and measuring tebipenem pivoxil related substances. According to the method, a chromatographic column adopts a C18 chromatographic column; a mobile phase is a mixed solution consisting of acetonitrile and a phosphate solution with the pH value being 3.0 to 6.0; column temperature is 38 to 40 DEG C; detection wavelength is 220 nm; flow velocity is 0.8 to 1.2 ml / min; gradient elution is performed by changing the ratio of the acetonitrile to the phosphate solution in the mobile phase. The method can effectively separate and measure six impurities of tebipenem pivoxil, has good separation degree and good peak shape, and can be applied to quality control of tebipenem pivoxil raw material medicines and tebipenem pivoxil medicine preparations.

Description

technical field [0001] The invention relates to the field of drug analysis, in particular to a high-performance liquid chromatography separation and determination method for related substances of the carbapenem antibiotic tibipenem. Background technique [0002] Tybipenem (compound of formula I), also known as tibipenem pivate, is a prodrug formed by the esterification of the C2 carboxylate of penem (carbapenem) drug tibipenem. It is produced by Wyeth A new type of oral carbapenem drug researched and developed by pharmaceutical companies. Tybipenem has a broad antibacterial spectrum, and it has stronger antibacterial activity than penicillin series and cephalosporin series against most clinically isolated strains. Compared with other injectable carbapenem antibiotics, Tybipenem also has Show the same degree or stronger antibacterial effect. Especially for PRSP (penicillin-resistant Streptococcus pneumoniae), MRSP (erythromycin-resistant Streptococcus pneumoniae) and Haemop...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/36
Inventor 尹志媛吕博雅柏江涛张广明
Owner 深圳万乐药业有限公司