Gas chromatography method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol and use thereof

A gas chromatographic analysis and ethyl acetate technology, which is applied in the fields of pharmaceutical synthesis and chemical industry, can solve the problems of not being environmentally friendly, time-consuming and labor-intensive, and waste of detection reagents, and achieve the effects of stable retention time, good separation effect and high accuracy.

Inactive Publication Date: 2016-07-27
JIANGSU WANBANG BIOPHARMLS +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

National standards have clear residue requirements for this, but the detection methods in the current national standards are all single detection methods for specific components, for example, they only detect n-heptane, so that in order to combine these four common The determination of the residual amount of all residual components requires four test operations, which is not only time-consuming and labor-intensive, but also wastes a lot of detection reagents, which does not meet the requirements of the modern era such as environmental friendliness

Method used

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  • Gas chromatography method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol and use thereof
  • Gas chromatography method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol and use thereof
  • Gas chromatography method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol and use thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Accurately weigh 0.1 g of the drug to be tested, put it in a headspace bottle, add 1 ml of dimethyl sulfoxide to dissolve it, seal it, and use it as the test solution.

[0029] In addition, accurately weigh the appropriate amount of isopropanol, ethyl acetate, isooctane and n-heptane, and add dimethyl sulfoxide to dilute to make a mixed solution containing 500 μg of isopropanol, 500 μg of ethyl acetate, and 500 μg of isooctane. , 500 μg of n-heptane reference substance solution.

Embodiment 2

[0031] The test solution and the reference solution were measured according to the residual solvent determination method (the second method of appendix VIIIP in the second part of the Chinese Pharmacopoeia 2010 edition), and the chromatograms of the reference solution were respectively obtained. figure 1 And the chromatogram of the test solution figure 2 . The test results are compared in the table below.

[0032]

Embodiment 3

[0034] Take 1mL of the test solution, put it in a 20ml headspace bottle, heat it at 80°C for 30 minutes, and then use the gas chromatography analysis method disclosed in the present invention to detect: the reagent sample is directly injected into the gas phase by manual injection. In the chromatograph, the injection volume is 1 μL. Using the DB-624 chromatographic column, set the initial temperature of the column temperature to 40°C, maintain it for 8 minutes, then raise the temperature to 220°C at a speed of 15°C per minute, and maintain it for 6 minutes; the temperature of the injection port is 250°C; the detector (FID ) temperature is 280°C; the carrier gas is nitrogen; record the chromatogram and get Figure 2 to Figure 6 .

[0035] Get 1mL of the reference substance solution, place it in a 20ml headspace bottle, heat it at 80°C for 30 minutes, and then use the gas chromatography analysis method disclosed in the present invention to detect: the test solution is directly ...

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Abstract

The invention relates to a gas chromatography analysis method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol. In order to obtain a gas phase detection method with simple operation, good peak shape, high column efficiency, good separation effect, good stability, good reproducibility, and common use for four reagents. We disclose a gas chromatographic analysis method, in which n-heptane, isooctane, ethyl acetate, and isopropanol are directly injected into the gas chromatograph, and nitrogen is used as a carrier gas to pass through 6% cyanopropylphenyl —94% dimethylpolysiloxane is used as a capillary chromatographic column as a stationary liquid, and the detected data is qualitatively and quantitatively analyzed by gas chromatography. By adopting the gas chromatography analysis method disclosed in the invention, the purity detection of n-heptane, isooctane, ethyl acetate and isopropanol can be performed conveniently and quickly. The main peak retention time of each reagent is stable, the peak shape is good, and the separation effect is good, which meets the requirements of residual reagent detection and quality control in drug synthesis or chemical synthesis.

Description

technical field [0001] The invention relates to the fields of medicine synthesis and chemical industry, in particular to a gas chromatography analysis method for simultaneously detecting n-heptane, isooctane, ethyl acetate and isopropanol. Background technique [0002] N-heptane, isooctane, ethyl acetate, and isopropanol are common organic residual solvents in pharmaceutical and chemical synthesis. National standards have clear residue requirements for this, but the detection methods in the current national standards are all single detection methods for specific components, for example, they only detect n-heptane, so that in order to combine these four common The determination of the residual amount of all residual components requires four test operations, which is not only time-consuming and labor-intensive, but also wastes a lot of detection reagents, which does not meet the requirements of the modern era such as environmental friendliness. Contents of the invention ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 王飞林彬刘跃跃乔德水高雪芹
Owner JIANGSU WANBANG BIOPHARMLS
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