CN112730646A - Method for measuring content of kerosene impurities - Google Patents

Method for measuring content of kerosene impurities Download PDF

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CN112730646A
CN112730646A CN202011433014.4A CN202011433014A CN112730646A CN 112730646 A CN112730646 A CN 112730646A CN 202011433014 A CN202011433014 A CN 202011433014A CN 112730646 A CN112730646 A CN 112730646A
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sample
kerosene
solution
reference substance
control
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邱伟杰
袁莉莉
陈铭辉
黄志云
刘明威
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Nanhai Beisha Pharmaceutical Co ltd
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Nanhai Beisha Pharmaceutical Co ltd
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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/86—Signal analysis

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Abstract

The invention discloses a method for measuring the content of kerosene impurities, which comprises the following steps: s1, respectively preparing a blank group sample, a control group sample and a test group sample; s2, respectively carrying out gas chromatography tests on the blank solvent sample, the reference group sample and the test group sample by using a gas chromatograph to obtain a chromatogram; calculating the absorption peak area A of kerosene in the sample of the control groupControlAnd the absorption peak area A of kerosene in the test group sampleSample (A)(ii) a And S3, calculating the content of kerosene in the sulfadiazine sample by using a formula. The invention can be used for measuring the content of kerosene in sulfadiazine, and the test result is reliable and has high accuracy. Can be suitable for most chemical analysis laboratories, and is convenient for popularization and use.

Description

Method for measuring content of kerosene impurities
Technical Field
The invention relates to the technical field of chemical detection, in particular to a method for determining the content of kerosene impurities.
Background
Sulfadiazine is an intermediate-effect sulfanilamide for treating systemic infection, has a wide antibacterial spectrum, has an inhibiting effect on most gram-positive bacteria and gram-negative bacteria, has a strong inhibiting effect on meningococcus, streptococcus pneumoniae, gonococcus and hemolytic streptococcus, and can permeate into cerebrospinal fluid through a blood brain barrier. Based on the limitation of the process level, the raw material for synthesizing sulfadiazine has part of kerosene impurities, and the part of kerosene impurities may exist in sulfadiazine after the sulfadiazine is synthesized, so that the kerosene impurities in the sulfadiazine and the derivatives thereof need to be measured.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the method for measuring the content of the kerosene impurities, which has novel technology, strong operability and high test accuracy.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for measuring the content of kerosene impurities comprises the following steps:
s1, respectively preparing a blank group sample, a control group sample and a test group sample; the blank group sample is prepared by the following process: weighing dimethyl sulfoxide with the volume of V in a headspace bottle, and capping and sealing to obtain a blank group sample; the preparation process of the control group sample is as follows: weighing mControlThe kerosene reference substance is diluted by dimethyl sulfoxide to obtain the concentration CControlThen weighing the reference substance solution to obtain a mass mSample (A)The sulfadiazine sample is placed in a headspace bottle, the reference substance solution is added into the headspace bottle to reach the volume V, and a reference group sample is prepared by covering and sealing; the test group samples were prepared as follows: weighing mSample (A)The sulfadiazine sample is placed in a headspace bottle, dimethyl sulfoxide is added into the headspace bottle to reach the volume V, and a test group sample is prepared by covering and sealing;
s2, respectively carrying out gas chromatography testing on the blank solvent sample, the reference group sample and the test group sample by using a gas chromatograph to obtain a chromatogram; screening corresponding absorption peaks of kerosene in a chromatogram by comparing chromatograms of a blank solvent sample, a reference sample and a test group sample, and calculating an absorption peak area A of the kerosene in the reference sampleControlAnd the absorption peak area A of kerosene in the test group sampleSample (A)；
S3, calculating the content of kerosene in the sulfadiazine sample by using the following formula:
Figure BDA0002827267890000011
wherein, CControlIs the mass-volume concentration of the kerosene reference solution in the reference sample, ASample (A)Is the chromatographic peak area of kerosene in the test solution, AControlM is the average value of the absorption peak area of kerosene in the control sampleSample (A)The sample is weighed.
Preferably, the preparation method of the control solution comprises the following steps: weighing mControlPlacing the kerosene reference substance in a 50ml measuring flask, diluting the kerosene reference substance to a scale with dimethyl sulfoxide, and shaking up to obtain a reference substance stock solution; taking 4ml of the reference substance stock solution, placing the reference substance stock solution in a 100ml volumetric flask, diluting the reference substance stock solution to the scale with dimethyl sulfoxide, and shaking up to prepare the reference substance solution.
The invention has the beneficial effects that: the method for measuring the content of the kerosene impurities can be used for detecting the content of the kerosene impurities in the sulfadiazine, and because the sulfadiazine and the kerosene impurities respectively have different absorption peaks in a gas chromatogram, the absorption peaks of the sulfadiazine and the kerosene impurities cannot be mutually overlapped, the sulfadiazine and the kerosene impurities can be analyzed and measured by a gas chromatograph, so that the content of the kerosene impurities can be calculated.
Detailed Description
The claimed solution will now be described in further detail with reference to specific embodiments.
Example one
The method for measuring the content of the kerosene impurities in the embodiment. The method comprises the following steps:
s1, respectively preparing a blank group sample, a control group sample and a test group sample.
The blank group of samples was prepared as follows: a blank sample was prepared by weighing 5ml volume of dimethyl sulfoxide into a 20ml headspace bottle and sealing with a cap.
The control sample was prepared as follows: weighing a kerosene reference substance with the mass of 0.1g, placing the kerosene reference substance into a 50ml measuring bottle, diluting the kerosene reference substance to a scale with dimethyl sulfoxide, and shaking up to obtain a reference substance stock solution; taking 4ml of the reference substance stock solution, placing the reference substance stock solution in a 100ml volumetric flask, diluting the reference substance stock solution to the scale with dimethyl sulfoxide, and shaking up to prepare the reference substance solution.
And then weighing a sulfadiazine sample with the mass of 2g, placing the sulfadiazine sample into a headspace bottle, adding the reference solution into the headspace bottle to the volume of 5ml, and covering and sealing to obtain a reference group sample.
The test group samples were prepared as follows: weighing a sulfadiazine sample with the mass of 2g, placing the sulfadiazine sample into a headspace bottle, adding dimethyl sulfoxide into the headspace bottle to the volume of 5ml, and covering and sealing to obtain a test group sample.
S2, respectively carrying out gas chromatography testing on the blank solvent sample, the reference group sample and the test group sample by using a gas chromatograph to obtain a chromatogram; in this example, the parameters of the gas chromatograph are shown in the following table:
Figure BDA0002827267890000021
Figure BDA0002827267890000031
screening the corresponding absorption peak of the kerosene in the chromatogram by comparing the chromatograms of the blank solvent sample, the reference sample and the test group sample, and calculating the absorption peak area A of the kerosene in the reference sampleControlAnd the absorption peak area A of kerosene in the test group sampleSample (A)。
S3, calculating the content of kerosene in the sulfadiazine sample by using the following formula:
Figure RE-GDA0002989010860000032
wherein, CControlIs the mass-volume concentration of the kerosene reference solution in the reference sample, ASample (A)Coal in solution for test articleChromatographic Peak area of oil, AControlM is the average value of the absorption peak area of kerosene in the control sampleSample (A)The sample is weighed.
Example two
In the method for determining the content of kerosene impurities in this embodiment, the sulfadiazine derivative in this embodiment includes sulfadiazine or sulfadimidine sodium. The method comprises the following steps:
s1, respectively preparing a blank group sample, a control group sample and a test group sample.
The blank group of samples was prepared as follows: a blank sample was prepared by weighing 1ml volume of dimethyl sulfoxide into a 20ml headspace bottle and sealing with a cap.
The control sample was prepared as follows: weighing a kerosene reference substance with the mass of 0.1g, placing the kerosene reference substance into a 50ml measuring bottle, diluting the kerosene reference substance to a scale with dimethyl sulfoxide, and shaking up to obtain a reference substance stock solution; taking 4ml of the reference substance stock solution, placing the reference substance stock solution in a 100ml volumetric flask, diluting the reference substance stock solution to the scale with dimethyl sulfoxide, and shaking up to prepare the reference substance solution.
And then weighing a sulfadiazine sample with the mass of 2g, placing the sulfadiazine sample into a headspace bottle, adding the reference solution into the headspace bottle to the volume of 1ml, and covering and sealing to obtain a reference group sample.
The test group samples were prepared as follows: weighing a sulfadiazine sample with the mass of 2g, placing the sulfadiazine sample into a headspace bottle, adding dimethyl sulfoxide into the headspace bottle to the volume of 1ml, and covering and sealing to obtain a test group sample.
S2, respectively carrying out gas chromatography testing on the blank solvent sample, the reference group sample and the test group sample by using a gas chromatograph to obtain a chromatogram; in this example, the parameters of the gas chromatograph are shown in the following table:
Figure BDA0002827267890000033
Figure BDA0002827267890000041
screening the corresponding absorption peak of the kerosene in the chromatogram by comparing the chromatograms of the blank solvent sample, the reference sample and the test group sample, and calculating the absorption peak area A of the kerosene in the reference sampleControlAnd the absorption peak area A of kerosene in the test group sampleSample (A)。
S3, calculating the content of kerosene in the sulfadiazine sample by using the following formula:
Figure RE-GDA0002989010860000042
wherein, CControlIs the mass-volume concentration of the kerosene reference solution in the reference sample, ASample (A)Is the chromatographic peak area of kerosene in the test solution, AControlM is the average value of the absorption peak area of kerosene in the control sampleSample (A)The sample is weighed.
The testing method for the content of the kerosene impurities is verified and tested to verify the accuracy of the testing method, and the testing method for the kerosene residue in sulfadiazine verifies the specificity, linearity, accuracy, precision, detection limit and quantitative limit.
And (3) specificity test: in each verification item, the blank solution has no interference at the peak appearance time of the reference, and the sample has no interference at the peak appearance time of the reference.
And (3) linear testing:
preparing a linear solution, transferring the reference solution into a 50ml volumetric flask, and adding dimethyl sulfoxide to dilute to a scale mark to obtain the linear solution. Weighing 2.0g of sulfadiazine sample, precisely weighing, placing in a 20ml headspace bottle, transferring 5.0ml of linear solution into the 20ml headspace bottle, and sealing with a cover to obtain a sample test solution. Wherein the linear concentrations are as follows:
Figure BDA0002827267890000043
the linear solutions of each concentration were injected into 2 needles and the average peak area was calculated. And (3) performing linear regression analysis by taking the concentration of the kerosene as an abscissa and the peak area as an ordinate, and calculating a correlation coefficient.
The results are shown in the following table:
Figure BDA0002827267890000051
and (3) testing accuracy:
and precisely adding a proper amount of reference substance solution into the test solution by adopting a standard adding recovery method to respectively prepare three accurate test solutions with three concentrations.
Preparing an accurate solution: the control solution was removed and placed in a 50ml volumetric flask (the volume of the control stock solution was removed to prepare the accuracy solution according to the table below), and then diluted to the scale with dimethyl sulfoxide to obtain control solutions of different concentrations. Weighing 2.0g of sulfadiazine sample, precisely weighing, placing in a 20ml headspace bottle, transferring 5.0ml of reference solution with corresponding concentration into the 20ml headspace bottle, sealing with a cover, and using as a sample injection test solution. (the concentrations at each accuracy are shown in the table below). Three concentrations of the exact solution were prepared, each in triplicate, and the results are given in the following table.
Figure BDA0002827267890000052
And (3) testing precision:
repeatability: according to the preparation method of the solutions with the accuracy A0 and A2, 1 part of the solution with the accuracy A0 and 6 parts of the solution with the accuracy A2 are prepared, 2 needles are injected into the solution with the accuracy A0, and 1 needle is injected into each solution with the accuracy A2.
Intermediate precision: on different days, 1 part of the accuracy A0 solution and 6 parts of the accuracy A2 solution were reconstituted by another experimenter according to a repetitive preparation method, 2 needles were injected with the accuracy A0 solution, and 1 needle was injected with each of the accuracy A2 solutions.
The results are shown in the following table:
Figure BDA0002827267890000061
and (3) quantitative limit testing:
transferring 1ml of the reference substance solution, placing the reference substance solution in a 50ml volumetric flask, and adding dimethyl sulfoxide to dilute the reference substance solution to a scale mark to obtain the reference substance test solution. The control test solution 5.0ml was removed in a 20ml headspace bottle, capped and sealed as a sample test solution. (concentration about 40. mu.g/ml, corresponding to a kerosene content of about 100ppm in the sample) 6 parts of each solution were prepared.
The results are shown in the following table:
Figure BDA0002827267890000062
remarking: and the S/N value is the minimum value of the three detected substance peaks.
Testing the detection limit:
0.3ml of the control solution is removed and placed in a 50ml volumetric flask, and dimethyl sulfoxide is added to dilute the solution to the scale, so that the sensitive solution is obtained. 5.0ml of the sensitivity solution was removed in a 20ml headspace bottle, capped and sealed as a sample test solution. 3 parts of solution are prepared separately. (concentration about 12. mu.g/ml, corresponding to a kerosene content of about 30ppm in the sample).
The results are shown in the following table:
Figure BDA0002827267890000071
remarking: and the S/N value is the minimum value of the three detected substance peaks.
And (3) sample detection testing:
the results of three batches of sulfadiazine samples tested by the above method are as follows:
Figure BDA0002827267890000072
the method for detecting the kerosene residue in sulfadiazine verifies that the detection method comprises specificity, linearity, accuracy, precision, detection limit and quantification limit, and the verification experiment result meets the preset limit, so that the method meets the detection requirement.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to limit the present invention in any way. Those skilled in the art can make many changes and modifications to the invention, and equivalents thereof, without departing from the scope of the invention, by applying the teachings disclosed above. Therefore, equivalent variations made according to the idea of the present invention should be covered within the protection scope of the present invention without departing from the content of the technical solution of the present invention.

Claims (2)

1. The method for measuring the content of the kerosene impurities is characterized by comprising the following steps of:
s1, respectively preparing a blank group sample, a control group sample and a test group sample;
the blank group of samples was prepared as follows: weighing dimethyl sulfoxide with the volume of V in a headspace bottle, and capping and sealing to obtain a blank group sample;
the control sample was prepared as follows: weighing mControlThe kerosene reference substance is diluted by dimethyl sulfoxide to obtain the concentration CControlThen weighing the reference substance solution to obtain a mass mSample (A)The sulfadiazine sample is placed in a headspace bottle, the reference substance solution is added into the headspace bottle to reach the volume V, and a reference group sample is prepared by covering and sealing;
the test group samples were prepared as follows: weighing mSample (A)The sulfadiazine sample is placed in a headspace bottle, dimethyl sulfoxide is added into the headspace bottle to reach the volume V, and a test group sample is prepared by covering and sealing;
s2, respectively carrying out gas chromatography test on the blank solvent sample, the reference group sample and the test group sample by using a gas chromatograph to obtain a chromatogram, screening corresponding absorption peaks of kerosene in the chromatogram by comparing the chromatograms of the blank solvent sample, the reference sample and the test group sample, and calculating an absorption peak area A of the kerosene in the reference sampleControlAnd the absorption peak area A of kerosene in the test group sampleSample (A)；
S3, calculating the content of kerosene in the sulfadiazine sample by using the following formula:
Figure RE-FDA0002989010850000011
wherein, CControlIs the mass-volume concentration of the kerosene reference solution in the reference sample, ASample (A)Is the chromatographic peak area of kerosene in the test sample solution, AControlM is the average value of the absorption peak area of kerosene in the control sampleSample (A)The sample is weighed.
2. The method for determining the impurity content of kerosene according to claim 1, wherein: the preparation method of the reference substance solution comprises the following steps: weighing mControlPlacing the kerosene reference substance in a 50ml measuring flask, diluting the kerosene reference substance to a scale with dimethyl sulfoxide, and shaking up to obtain a reference substance stock solution; taking 4ml of the reference substance stock solution, placing the reference substance stock solution in a 100ml volumetric flask, diluting the reference substance stock solution to the scale with dimethyl sulfoxide, and shaking up to prepare the reference substance solution.
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CN102128892A (en) * 2010-12-22 2011-07-20 宝钢集团新疆八一钢铁有限公司 Improved gas chromatographic measurement method for naphthalene content in coal tar
CN102253149A (en) * 2011-05-05 2011-11-23 辽宁省刑事科学技术研究所 Method for synchronously analyzing combustion residues of hydrocarbons and sulfides in fire on-site combustion improver

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Publication number Priority date Publication date Assignee Title
CN101782559A (en) * 2010-02-21 2010-07-21 河南海星化工科技有限公司 Method for rapidly detecting component content of coal tar
CN102128892A (en) * 2010-12-22 2011-07-20 宝钢集团新疆八一钢铁有限公司 Improved gas chromatographic measurement method for naphthalene content in coal tar
CN102253149A (en) * 2011-05-05 2011-11-23 辽宁省刑事科学技术研究所 Method for synchronously analyzing combustion residues of hydrocarbons and sulfides in fire on-site combustion improver

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