CN115060833A - Detection method for determining residual drug in propylthiouracil by gas chromatography - Google Patents
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Abstract
The invention discloses a detection method for determining residual drugs in propylthiouracil by gas chromatography, which comprises the following steps: the residual medicine is acetic acid, and the detection method comprises the following steps: a preparing solution, comprising: stock solution: preparing acetic acid with concentration of 10000 ug/ml; standard solution: acetic acid concentration: 1000 ug/ml; test solution preparation: weighing 1.0g of sample to be tested in a 5ml volumetric flask, and metering the volume of the prepared solution by using N, N-dimethylformamide; and B, detecting by using a gas chromatograph, wherein a chromatographic column adopts DB-624, 30m x 0.53mm x 3.0 m, carrier gas is nitrogen, the flow rate of the carrier gas is 4.0ml/min, the temperature of a sample injector is 200 ℃, the temperature of a detector is 250 ℃, the column temperature: and (3) keeping the temperature at 45 ℃ for 5min, then increasing the temperature to 180 ℃ at the speed of 40 ℃/min, then keeping the temperature for 6min, dividing the flow ratio to be 20:1, and detecting the prepared solution in the step A by adopting the gas chromatograph and the set indexes, wherein the sample injection volume is 1L. The invention realizes the detection of residual acetic acid in propylthiouracil, and the prepared medicine meets the quality regulation.
Description
Technical Field
The invention relates to the technical field of residual solvents, in particular to a detection method for determining residual medicines in propylthiouracil by using a gas chromatography.
Background
The propylthiouracil is used for treating adult hyperthyroidism, the initial dose is generally 300mg per day, the dosage is 150-400 mg according to the severity of disease, and the maximum dosage is 600mg per day. Propylthiouracil is an antithyroid agent and its mechanism of action is the inhibition of thyroxine. Common adverse reactions include headache, vertigo, arthralgia, swollen salivary glands and lymph nodes and gastrointestinal tract reaction; there are also allergic reactions such as rash and drug fever, and some rashes may develop into exfoliative dermatitis.
However, the drug effect of propylthiouracil is affected to a certain extent by excessive residual acetic acid-containing drug in propylthiouracil produced at present.
Therefore, the residual content of the solvent in the propylthiouracil needs to be detected, and no gas chromatography is reported for detecting the residual acetic acid content in propylthiouracil.
Disclosure of Invention
The present invention addresses one or more of the above-mentioned problems of the prior art by providing a method for detecting residual drug in propylthiouracil by gas chromatography.
According to a first aspect of the present invention, there is provided a detection method for detecting a residual drug in propylthiouracil by gas chromatography, wherein the residual drug is acetic acid, the detection method comprising the steps of:
a preparing solution, comprising:
stock solution: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, and carrying out constant volume with N, N-dimethylformamide to obtain the acetic acid concentration: 10000 ug/ml;
standard solution: preparation to transfer 1ml of stock solution to a 10ml volumetric flask, constant volume with N, N-dimethylformamide, acetic acid concentration: 1000 ug/ml; test solution preparation: weighing 1.0g of a sample to be tested in a 5ml volumetric flask, and performing constant volume by using N, N-dimethylformamide;
b, detecting by using a gas chromatograph, wherein a chromatographic column adopts DB-624, 30m x 0.53.53 mm x 3.0 m, carrier gas is nitrogen, the flow rate of the carrier gas is 4.0ml/min, the temperature of a sample injector is 200 ℃, the temperature of a detector is 250 ℃, the column temperature: and (3) keeping the temperature at 45 ℃ for 5min, then increasing the temperature to 180 ℃ at the speed of 40 ℃/min, keeping the temperature for 6min again, carrying out detection on the prepared solution in the step A by adopting the gas chromatograph and the set indexes, wherein the split ratio is 20:1, and the sample injection volume is 1L. In some possible implementations, the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index includes:
and repeating the sampling of 6 needles with the same standard concentration, obtaining the RSD value of each solvent peak area of the standard solution in the obtained chromatogram, and judging whether the RSD value is less than a preset value, namely the RSD is less than or equal to 10%.
In some possible implementations, the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index includes: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 150ul of the solution into the 100ml volumetric flask, metering the volume with N, N-dimethylformamide, detecting by adopting the method in the step B, obtaining the limit of detection LOD of the acetic acid, and judging whether the limit of detection LOD meets the standard or not.
In some possible implementations, the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index includes: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 400ul of the solution into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide, detecting by adopting the method in the step B, obtaining the quantitative limit LOQ of the acetic acid, and judging whether the quantitative limit LOQ meets the standard or not.
In some possible implementations, the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index includes: preparing a solution: preparing solutions with acetic acid concentrations of 10003ug/ml, 10004ug/ml and 9999ug/ml respectively, transferring a certain amount of solutions from the three solutions to prepare 6 concentrations for sample injection, and preparing LOQ concentration, 20% index concentration, 50% index concentration, 80% index concentration, 100% index concentration and 150% index concentration, wherein each concentration is divided into three parts;
and B, detecting each concentration of the prepared solution by adopting the method in the step B, so as to obtain a linear equation of the acetic acid and a regression coefficient of the linear equation.
The invention has the beneficial effects that:
by adopting the method for detecting the residual medicine in the propylthiouracil by the gas chromatography, the accurate measurement and analysis of the residual acetic acid in the propylthiouracil can be accurately realized, the method comprises a quantitative limit and a detection limit, is rapid and accurate, the monitoring efficiency is improved, and powerful data support is provided for the improvement of medicines.
Drawings
FIG. 1 is a graph showing the relationship of the linear equation of acetic acid detected by a detection method for measuring a residual drug in propylthiouracil by gas chromatography.
With the foregoing drawings in mind, certain embodiments of the disclosure have been shown and described in more detail below. These drawings and written description are not intended to limit the scope of the disclosed concepts in any way, but rather to illustrate the concepts of the disclosure to those skilled in the art by reference to specific embodiments.
Detailed Description
The technical scheme of the application is further explained in detail with reference to the attached drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Some embodiments of the invention are described in detail below with reference to the accompanying drawings. In case of conflict, features of the following embodiments and embodiments may be combined with each other, and details of the same or similar concepts or processes may not be repeated in some embodiments.
Example one
The embodiment of the invention provides a detection method for determining residual drugs in propylthiouracil by using a gas chromatography, wherein the residual drugs are acetic acid; the detection method comprises the following steps:
A. preparing a solution comprising:
stock solution: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, and carrying out constant volume with N, N-dimethylformamide to obtain the acetic acid concentration: 10000 ug/ml;
standard solution: preparation to transfer 1ml of stock solution to a 10ml volumetric flask, constant volume with N, N-dimethylformamide, acetic acid concentration: 1000 ug/ml; test solution preparation: weighing 1.0g of a sample to be tested in a 5ml volumetric flask, and performing constant volume by using N, N-dimethylformamide;
B. detecting by using a gas chromatograph, wherein the model of the gas chromatograph adopts Agilent 7890B, and the instrument is corrected to meet the specification, wherein a chromatographic column adopts DB-624, 30m x 0.53mm x 3.0 m, carrier gas is nitrogen, the flow rate of the carrier gas is 4.0ml/min, the temperature of a sample injector is 200 ℃, the temperature of a detector is 250 ℃, and the column temperature: keeping the temperature at 45 ℃ for 3min, then increasing the temperature to 180 ℃ at the speed of 40 ℃/min, keeping the temperature for 6min again, performing split ratio of 20:1, and detecting the solution in the step A by adopting the gas chromatograph and setting indexes, wherein the sample injection volume is 1L;
C. and repeating the sampling of 6 needles with the same standard concentration, obtaining the RSD value of each solvent peak area of the standard solution in the obtained chromatogram, judging whether the RSD value is less than a preset value, namely the RSD is less than or equal to 10%, and detecting results are shown in table 1, so that the RSD of the solvent peak area of 6 times of sampling of 6 needles by repeating the standard solution is less than or equal to 10% as can be seen from the table, and the requirement on system adaptability is met.
TABLE 1
| Sample introduction sequence | Retention time | Area of acetic acid peak |
| Concentration of Standard solution (ug/ml) | — | 1000.1 |
| 1 | 3.070 | 242.37 |
| 2 | 3.069 | 241.37 |
| 3 | 3.068 | 242.21 |
| 4 | 3.074 | 254.70 |
| 5 | 3.083 | 261.70 |
| 6 | 3.080 | 260.79 |
| Average | 3.074 | 250.52 |
| RSD% | 0.21 | 3.86 |
However, for the potential residual organic solvent, a detection limit LOD and a quantification limit LOQ, which are determined according to the signal-to-noise ratio method, are also required. The limit of quantitation is the lowest amount or concentration at which the analyte (or component to be detected) in the sample can be quantified, and the limit of detection LOD is the lowest concentration or lowest amount at which the component to be detected can be detected under the specified experimental conditions. The lowest concentration or percentage that can be reliably detected is calculated by comparing the measured signal with the signal (baseline noise) of the blank, which is a sample diluted to a low concentration in a stock solution of known concentration, and the detection limit is determined by the sample concentration corresponding to a signal-to-noise ratio (S/N) of about 3 in this example.
Specifically, the detection limit detection specifically comprises: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 150ul of the solution into the 100ml volumetric flask, metering the volume with N, N-dimethylformamide, detecting by adopting the method in the step 2, obtaining the detection limit LOD of the acetic acid and judging whether the detection limit LOD meets the standard or not; as shown in table 2, the detection limit of acetic acid was obtained. As can be seen from Table 2, the limit of detection of acetic acid in this method is about 1.5ug/ml, corresponding to 7.5ppm of the sample, and meets the standard for a concentration that specifies a signal-to-noise ratio of 3: 1. Thereby, the detection limit of the sample to be measured is detected.
TABLE 2
| Sample introduction sequence | Substance(s) | Concentration (ug/ml) | Peak area | Peak height | Signal-to-noise ratio (S/N) | Content (ppm) corresponding to sample concentration |
| Blank space | — | — | — | — | — | — |
| Detection limit 1 | Acetic Acid (AA) | 1.5005 | 0.56 | 0.28 | 3.87 | 7.502 |
| Detection limit 2 | Acetic acid | 1.5004 | 0.55 | 0.26 | 3.56 | 7.502 |
| Detection limit 3 | Acetic acid | 1.5005 | 0.56 | 0.29 | 3.92 | 7.502 |
| Average | — | 1.5004 | 0.56 | 0.28 | 3.78 | 7.502 |
| RSD% | — | — | 1.15 | 5.07 | — | — |
For the quantitative limit, the quantitative limit is determined at a sample concentration corresponding to a signal-to-noise ratio (S/N) of about 10. The quantitative limit detection specifically comprises the following steps: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 400ul of the solution into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide, detecting by adopting the method in the step 2, obtaining the quantitative limit LOQ of the acetic acid and judging whether the quantitative limit LOQ meets the standard or not.
As can be seen from Table 3, the limit of quantitation of acetic acid is about 4ug/ml, which is equivalent to 20ppm of the sample concentration, the peak area RSD of 6 injections is 0.66%, the peak area RSD of 6 injections is 4.96%, and the detection result meets the standard. The method can be used for detecting the limit of quantification of the acetic acid.
TABLE 3
Preferably, the method further comprises the step of carrying out linear detection on the acetic acid to obtain a linear regression equation of the acetic acid, wherein a correlation coefficient R is more than or equal to 0.996, and the RSD of different concentration peak areas is less than or equal to 10 percent
The method specifically comprises the following steps: preparation of stock solutions: preparing solutions with acetic acid concentrations of 10003ug/ml, 10004ug/ml and 9999ug/ml, respectively preparing 6 concentrations of sample injection from the three solutions, and preparing three solutions with LOQ concentration, index concentration of 20%, index concentration of 50%, index concentration of 80%, index concentration of 100% and index concentration of 150%, wherein each concentration is three, so that 18 solutions are obtained;
detecting each concentration of the prepared solution by adopting the method in the step B, thereby obtaining a linear equation of the acetic acid and a regression coefficient of the linear equation, wherein the method comprises the following steps: obtaining LOQ concentration: the resulting stock solution was transferred in an amount of 1ml to a 10ml volumetric flask, 400ul of the solution was transferred to a 100ml volumetric flask and the volume was determined by N, N-dimethylformamide.
The concentration of each index: specifically, the solutions with index concentration of 20%, index concentration of 50%, index concentration of 80%, index concentration of 100% and index concentration of 150% can be obtained by transferring stock solutions of 0.2ml, 0.5ml, 0.8ml, 1ml and 1.5ml to 10ml volumetric flasks respectively, and performing constant volume with N, N-dimethylformamide. The acetic acid linearity test results were obtained by using the above step 2, and the test results are shown in the following table. Specifically, a gas chromatograph is adopted for detection, the model of the gas chromatograph adopts Agilent 7890B, the instrument is corrected to meet the specification, wherein a chromatographic column adopts DB-624, 30mx 0.53mm x 3.0 m, carrier gas is nitrogen, the flow rate of the carrier gas is 4.0ml/min, the temperature of a sample injector is 200 ℃, the temperature of a detector is 250 ℃, the column temperature: keeping the temperature at 45 ℃ for 3min, then increasing the temperature to 180 ℃ at a speed of 40 ℃/min, keeping the temperature for 6min again, carrying out a split ratio of 20:1, and detecting 18 prepared solutions by adopting the gas chromatograph and setting indexes, wherein the sample injection volume is 1 mu L. From this, it is obtained from table 4 that the acetic acid linear equation is y =0.2181X-2.9577, the regression coefficient R is 0.9997, the linear equation is inclined to 0.2181, the y-intercept is-2.9577, the linear regression coefficient R is 0.9997, and it can be known from the linear equation that the concentration range is quantitatively limited to 150% of the injection concentration, namely 4ug/ml-1500ug/ml (20 ppm-7500 ppm).
TABLE 4
| Sample introduction sequence | Concentration (ug/ml) | Average concentration (ug/ml) | Peak area | Average peak area | RSD≤10.0% | Approximately corresponding to the concentration of the sample |
| 1 | 4.0012 | 4.0008 | 1.11 | 1.09 | 2.11 | 20ppm |
| 2 | 4.0016 | 4.0008 | 1.07 | 1.09 | 2.11 | 20ppm |
| 3 | 3.9996 | 4.0008 | 1.08 | 1.09 | 2.11 | 20ppm |
| 4 | 200.06 | 200.04 | 38.87 | 38.93 | 0.55 | 1000ppm |
| 5 | 200.08 | 200.04 | 38.76 | 38.93 | 0.55 | 1000ppm |
| 6 | 199.98 | 200.04 | 39.17 | 38.93 | 0.55 | 1000ppm |
| 7 | 500.15 | 500.10 | 105.01 | 105.44 | 0.44 | 2500ppm |
| 8 | 500.20 | 500.10 | 105.94 | 105.44 | 0.44 | 2500ppm |
| 9 | 499.95 | 500.10 | 105.37 | 105.44 | 0.44 | 2500ppm |
| 10 | 800.24 | 800.16 | 165.33 | 168.99 | 3.56 | 4000ppm |
| 11 | 800.32 | 800.16 | 175.93 | 168.99 | 3.56 | 4000ppm |
| 12 | 799.92 | 800.16 | 165.72 | 168.99 | 3.56 | 4000ppm |
| 13 | 1000.30 | 1000.20 | 214.26 | 214.99 | 0.34 | 5000ppm |
| 14 | 1000.40 | 1000.20 | 214.97 | 214.99 | 0.34 | 5000ppm |
| 15 | 999.90 | 1000.20 | 215.73 | 214.99 | 0.34 | 5000ppm |
| 16 | 1500.45 | 1500.30 | 327.65 | 326.08 | 0.53 | 7500ppm |
| 17 | 1500.60 | 1500.30 | 326.36 | 326.08 | 0.53 | 7500ppm |
| 18 | 1499.85 | 1500.30 | 324.22 | 326.08 | 0.53 | 7500ppm |
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
What has been described above are merely some embodiments of the present invention. It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (5)
1. A detection method for determining residual drugs in propylthiouracil by gas chromatography is characterized in that the residual drugs are acetic acid, and the detection method comprises the following steps:
A. preparing a solution comprising:
stock solution: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, and carrying out constant volume with N, N-dimethylformamide to obtain the acetic acid concentration: 10000 ug/ml;
standard solution: preparation to transfer 1ml of stock solution to a 10ml volumetric flask and to volume with N, N-dimethylformamide, acetic acid concentration: 1000 ug/ml; test solution preparation: weighing 1.0g of a sample to be tested in a 5ml volumetric flask, and fixing the volume by using N, N-dimethylformamide;
B. and (3) detecting by using a gas chromatograph, wherein a chromatographic column adopts DB-624, 30m x 0.53mm x 3.0 m, carrier gas is nitrogen, the flow rate of the carrier gas is 4.0ml/min, the temperature of a sample injector is 200 ℃, the temperature of a detector is 250 ℃, the column temperature: and (3) keeping the temperature at 45 ℃ for 5min, then increasing the temperature to 180 ℃ at the speed of 40 ℃/min, keeping the temperature for 6min again, carrying out detection on the prepared solution in the step A by adopting the gas chromatograph and the set indexes, wherein the split ratio is 20:1, and the sample injection volume is 1L.
2. The method for detecting the residual drug in the propylthiouracil by gas chromatography according to claim 1, wherein the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index comprises the following steps:
and repeating the sampling of 6 needles with the same standard concentration, obtaining the RSD value of each solvent peak area of the standard solution in the obtained chromatogram, and judging whether the RSD value is less than a preset value, namely the RSD is less than or equal to 10%.
3. The method for detecting the residual drug in the propylthiouracil by gas chromatography according to claim 1, wherein the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index comprises the following steps: weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume with N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 150ul of the solution into the 100ml volumetric flask, metering the volume with N, N-dimethylformamide, detecting by adopting the method in the step B, obtaining the limit of detection LOD of the acetic acid, and judging whether the limit of detection LOD meets the standard or not.
4. The method for detecting the residual medicine in the propylthiouracil by the gas chromatography according to claim 1, wherein the step B of detecting the prepared solution in the step A by using the gas chromatograph and the set indexes comprises the following steps: and B, weighing 1g of acetic acid, adding the acetic acid into a 100ml volumetric flask, metering the volume by using N, N-dimethylformamide to obtain a solution, transferring 1ml of the solution into a 10ml volumetric flask, transferring 400ul of the solution into a 100ml volumetric flask, metering the volume by using N, N-dimethylformamide, detecting by adopting the method in the step B, obtaining the quantitative limit LOQ of the acetic acid, and judging whether the quantitative limit LOQ meets the standard or not.
5. The method for detecting the residual drug in the propylthiouracil by gas chromatography according to claim 1, wherein the step B of detecting the prepared solution in the step a by using the gas chromatograph and the set index comprises the following steps: preparing a solution: preparing solutions with acetic acid concentrations of 10003ug/ml, 10004ug/ml and 9999ug/ml respectively, transferring a certain amount of solutions from the three solutions to prepare 6 concentrations for sample injection, and preparing LOQ concentration, 20% index concentration, 50% index concentration, 80% index concentration, 100% index concentration and 150% index concentration, wherein each concentration is divided into three parts;
and B, detecting each concentration of the prepared solution by adopting the method in the step B, so as to obtain a linear equation of the acetic acid and a regression coefficient of the linear equation.
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Application publication date: 20220916 |