Determination method of residual ethanol in amoxicillin and clavulanate potassium preparation

A technology of amoxicillin-clavulanate potassium and detection method, applied in the field of drug analysis, can solve the problems of human injury, patient irritation, poor stability, etc., and achieve the effects of stable and reliable results, wide linear range and high sensitivity

Active Publication Date: 2020-07-31
LUNAN PHARMA GROUP CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The existence of excess ethanol will cause great damage to the human body, stimulate the patient, usually cause pain, and affect the joint movement and the function of other organs. The detection method provided by the current technology is not sensitive, and The defect of poor stability requires further research to explore a fast, sensitive and stable detection method to facilitate and accurately analyze the residual amount of ethanol in amoxicillin-clavulanate potassium and improve the quality of the preparation

Method used

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  • Determination method of residual ethanol in amoxicillin and clavulanate potassium preparation
  • Determination method of residual ethanol in amoxicillin and clavulanate potassium preparation
  • Determination method of residual ethanol in amoxicillin and clavulanate potassium preparation

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Experimental program
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Effect test

Embodiment 1

[0048] Embodiment 1 specificity test

[0049] Instruments and conditions: Shimadzu GC-2010PLUC gas chromatograph; DANI HSS86.50 PLUS headspace instrument; FID detector; chromatographic column SH-TRS624 (30m×0.52mm, 3μm); carrier gas is nitrogen; inlet temperature 200 ℃; detector temperature 250 ℃; column flow rate 3ml / min; split ratio 10:1; water as solvent; headspace bottle equilibrium temperature 80 ℃, headspace time: 30 minutes; Maintain for 8 minutes, then raise the temperature to 200°C at a rate of 30°C / min, and maintain for 10 minutes.

[0050] experiment procedure:

[0051] 1. Take water as the blank solvent, accurately measure 2ml, put it in a 20ml headspace bottle, and seal it. Headspace sampling, record chromatogram, see attached figure 1 .

[0052] 2. Accurately weigh 78.43mg of amoxicillin raw material, put it in a 20ml headspace bottle, add 2ml of water, seal, shake well, and use it as amoxicillin raw material test solution. Headspace sampling, record chromat...

Embodiment 2

[0058] Embodiment 2 quantification limit and detection limit test

[0059] Instruments and conditions: Shimadzu GC-2010PLUC gas chromatograph; DANI HSS86.50 PLUS headspace instrument; FID detector; chromatographic column SH-TRS624 (30m×0.52mm, 3μm); carrier gas is nitrogen; inlet temperature 200 ℃; detector temperature 250 ℃; column flow rate 3ml / min; split ratio 10:1; water as solvent; headspace vial equilibrium temperature 80 ℃, headspace time: 30 minutes; Maintain for 8 minutes, then raise the temperature to 200°C at a rate of 30°C / min, and maintain for 10 minutes.

[0060] experiment procedure:

[0061] 1. Take an appropriate amount of ethanol reference substance and dilute it with water to a solution containing 5.03 μg of absolute ethanol per 1 ml as the limit of quantitation solution. Precisely measure 2ml, put it in a 20ml headspace bottle, seal it, measure it according to the law, record the chromatogram, see the attached Figure 6 .

[0062] Depend on Figure 6 I...

Embodiment 3

[0065] Embodiment 3 linear range test

[0066] Instruments and conditions: Shimadzu GC-2010PLUC gas chromatograph; DANI HSS86.50 PLUS headspace instrument; FID detector; chromatographic column SH-TRS624 (30m×0.52mm, 3μm); carrier gas is nitrogen; inlet temperature 200 ℃; detector temperature 250 ℃; column flow rate 3ml / min; split ratio 10:1; water as solvent; headspace vial equilibrium temperature 80 ℃, headspace time: 30 minutes; Maintain for 8 minutes, then raise the temperature to 200°C at a rate of 30°C / min, and maintain for 10 minutes.

[0067] experiment procedure:

[0068] Take an appropriate amount of ethanol reference substance, and prepare solutions containing 5.03 mg / ml, 100.54 mg / ml, 201.08 mg / ml, 502.70 mg / ml, 754.05 mg / ml, and 1005.40 mg / ml of ethanol with water respectively. Precisely measure 2ml, put it in a 20ml headspace bottle, seal it, detect according to the law, record the chromatogram, and the results are shown in Table 2.

[0069] The results show ...

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Abstract

The present invention discloses a method for detecting the ethanol residue content in an amoxicillin and clavulanate potassium preparation, and belongs to the technical field of drug analysis. The method is characterized in that: gas chromatography is used for detection; the injection mode is headspace injection, and nitrogen is used as carrier gas; an SH-TRS624 chromatographic column is used; thedetector type is a hydrogen flame ionization detector; and temperature programming is performed. According to the method provided by the present invention, the ethanol residue content in the amoxicillin and clavulanate potassium preparation, especially the amoxicillin and clavulanate potassium plate / dispersion tablet, can be effectively detected; the method has high sensitivity, a wide linear range, good durability, simple operations, and a stable and reliable result; and the method can be applied to the detection of ethanol residues in the production process of related preparation products,and provides strong guarantee for the quality of medicines.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular to a method for detecting residual ethanol in amoxicillin-clavulanate potassium preparations, in particular to a method for detecting residual ethanol in amoxicillin-clavulanate potassium preparations based on gas chromatography method. Background technique [0002] Potassium clavulanate has only weak antibacterial activity, but it can be firmly combined with most β-lactamases to form irreversible conjugates. It has an effect on the enzymes produced by a variety of Gram-negative bacteria, so it is an effective β-lactamase inhibitor. [0003] Amoxicillin, also known as amoxycillin or amoxycillin, is the most commonly used semi-synthetic penicillin-type broad-spectrum β-lactam antibiotic. It is a white powder with a half-life of about 61.3 minutes. Stable under acidic conditions, the gastrointestinal absorption rate reaches 90%. Amoxicillin has a strong bactericidal effect an...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor房兆营郭小为
OwnerLUNAN PHARMA GROUP CORPORATION