Method for detecting residual quantity of triethylamine in beta-lactam antibiotic

A detection method and technology of triethylamine, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of difficulty in liquid separation and sampling, inability to detect residual amount, and interference with triethylamine detection.

Active Publication Date: 2013-04-03
SICHUAN KELUN PHARMA RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0004] Although there are currently some reports in the literature on the determination of residual triethylamine in cephalosporin or macrolide antibiotics by headspace gas chromatography, it is impossible to detect the 0.032% limit without a thorough modification of the injection channel system (change to an inert pipeline) However, it is not easy to transform the pipeline of a complete set of precision instruments
There is also bibliographical report to measure directly after extracting triethylamine with chloroform in addition, but chloroform toxicity is bigger, and the pollution to operator and environment is all bigger, after chloroform extracts, chloroform layer is below, and liquid separation sampling is difficult, and chloroform peak position and The peak of triethylamine is approaching, and the high concentration of chloroform and residues are likely to interfere with the detection of trace triethylamine

Method used

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  • Method for detecting residual quantity of triethylamine in beta-lactam antibiotic
  • Method for detecting residual quantity of triethylamine in beta-lactam antibiotic
  • Method for detecting residual quantity of triethylamine in beta-lactam antibiotic

Examples

Experimental program
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Effect test

Embodiment 1

[0043] The mensuration of triethylamine residual amount in the cefotaxime sodium of embodiment 1

[0044] Sample information: Cefotaxime sodium, Guilin Dahua Pharmaceutical Co., Ltd., Guangxi Zhuang Autonomous Region, batch numbers: BD080701, BD080702, BD080703.

[0045] Agilent 6890N Network GC System;

[0046]Workstation: Agilent chemstation;

[0047] Agilent HP-5, 30m*0.32mm*0.25μm;

[0048] SPH-300 hydrogen generator, Beijing China HP;

[0049] XWK-Ⅲ oil-free air pump, Tianjin Huasheng Analytical Instrument Factory;

[0050] Balance: Sartorius ALC-210.4, ALC-210.3, Sartorius cp225D;

[0051] Toluene: Chengdu Kelong Chemical Reagent Factory, 070704, analytically pure;

[0052] 2mol / L sodium hydroxide solution: weigh 8g of sodium hydroxide, put it in a beaker, add an appropriate amount of water, stir to dissolve completely, add water to dilute to 100ml.

[0053] Test solution: Accurately weigh 1.0g of each of the 3 batches of samples, put them in a 20ml stoppered test ...

Embodiment 2

[0070] Embodiment 2: the mensuration of triethylamine residue in ceftriaxone sodium

[0071] Sample information: Ceftriaxone sodium, Guilin Dahua Pharmaceutical Co., Ltd., Guangxi Zhuang Autonomous Region, batch number: BD091201, BD091202, BD091203.

[0072] Agilent 6890N Network GC System;

[0073] Workstation: Agilent chemstation;

[0074] Chromatographic column: SE-52, 50m*0.5mm*0.5μm;

[0075] SPH-300 hydrogen generator, Beijing China HP;

[0076] XWK-Ⅲ oil-free air pump, Tianjin Huasheng Analytical Instrument Factory;

[0077] Balance: Sartorius ALC-210.4, ALC-210.3, Sartorius cp225D;

[0078] Toluene: Chengdu Kelong Chemical Reagent Factory, 070704, analytically pure;

[0079] 1mol / L potassium hydroxide solution: weigh 5.6g of sodium hydroxide, put it in a beaker, add an appropriate amount of water, stir to dissolve completely, add water to dilute to 100ml.

[0080] Test solution: Accurately weigh 0.5g of each of the 3 batches of samples, put them in a 10ml stopper...

Embodiment 3

[0096] Example 3: Determination of residual triethylamine in faropenem sodium

[0097] Sample information: Faropenem Sodium, Sichuan Kelun Pharmaceutical Co., Ltd., batch numbers: 090701, 090702, 090703.

[0098] Agilent 6890N Network GC System;

[0099] Workstation: Agilent chemstation;

[0100] Chromatographic column: Agilent HP-1, 20m*0.32mm*0.25μm;

[0101] SPH-300 hydrogen generator, Beijing China HP;

[0102] XWK-Ⅲ oil-free air pump, Tianjin Huasheng Analytical Instrument Factory;

[0103] Balance: Sartorius ALC-210.4, ALC-210.3, Sartorius cp225D;

[0104] Toluene: Chengdu Kelong Chemical Reagent Factory, 070704, analytically pure;

[0105] 5mol / L sodium hydroxide solution: weigh 20g of sodium hydroxide, put it in a beaker, add an appropriate amount of water, stir to dissolve completely, add water to dilute to 100ml.

[0106] Test solution: Accurately weigh 2.0g of each of the 3 batches of samples, put them in a 25ml stoppered test tube, add 20ml of water and 0.5ml...

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Abstract

The invention provides a method for detecting the residual quantity of triethylamine in beta-lactam antibiotic. The method comprises the step of detecting by using a gas chromatographic method. According to the method, toluene is used as an extracting solvent, and the residual quantity of the triethylamine can be effectively measured under appropriate chromatographic condition in match, so that a novel method which is simpler and more feasible in detecting the residual quantity of the triethylamine in the beta-lactam antibiotic is provided.

Description

technical field [0001] The invention relates to a method for detecting residual triethylamine in β-lactam antibiotics. Background technique [0002] Triethylamine is a widely used reagent in the synthesis of β-lactam antibiotics. It is highly irritating to the respiratory tract and can cause pulmonary edema and even death after inhalation. Relevant toxicological information: acute toxicity: LD50460mg / kg (rat oral), 570mg / kg (rabbit dermal); LC50 6000mg / m 3 , 2 hours (mouse inhalation); irritation: Rabbit eyes: 250μg (24 hours), severe irritation. Subacute and chronic toxicity: Rabbit inhalation 420mg / m 3 , 7 hours / time, 5 times a week, 6 weeks, see pulmonary congestion, hemorrhage, peribronchitis, myocardial degeneration, liver and kidney congestion, degeneration, and necrosis. Reproductive toxicity: The minimum toxic dose (TDL0) of rabbit oral administration: 6900μg / kg (1 to 3 days of pregnancy), which has an impact on development. In view of the safety of triethylamine...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/60
Inventor 赵忠琼余佳徐国熙李明杨蕾梁隆王利春沈鑫程志鹏
Owner SICHUAN KELUN PHARMA RES INST CO LTD
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