Method for detecting perfluorobromooctane in carrier with DSPC as pore-forming agent

Abstract

The invention discloses a method for detecting perfluorobromooctane in a carrier with distearoyl phosphatidylcholine as a pore-forming agent, and relates to the technical field of drug detection.The method comprises the steps that firstly, the carrier with DSPC as the pore-forming agent is pretreated, and a to-be-detected sample solution is obtained; then preparing a reference substance solution; analyzing and detecting the to-be-detected sample solution and the reference substance solution by adopting a gas chromatographic method, and calculating the content of perfluorobromooctane in the to-be-detected sample solution; according to the method for detecting the perfluorobromooctane in the carrier taking the DSPC as the pore-forming agent, the perfluorobromooctane with extremely low concentration can be detected by selecting a high-sensitivity detector and optimized chromatographic conditions, which is crucial for tracking and monitoring trace change of the perfluorobromooctane; through strict experimental design and quality control, the stability and reliability of the method are ensured, consistent analysis results can be provided at different times, among different operators and different devices, and the credibility of experimental results is improved.

Description

Technical Field

[0001] The invention relates to a drug detection technology, in particular to a method for detecting perfluorooctane bromide in a carrier using DSPC as a pore-forming agent. Background Art

[0002] Perfluorooctyl bromide (PFOB) is a perfluorinated compound with potential application value in many fields due to its unique physical and chemical properties. The carrier material is usually prepared from DSPC (distearoylphosphatidylcholine), calcium chloride and perfluorooctyl bromide in a certain proportion.

[0003] At present, the detection method of perfluorooctyl bromide cannot accurately detect the content of perfluorooctyl bromide in samples with complex components, and the existing detection method is mainly for the test solution of direct injection, and is not suitable for the detection of perfluorooctyl bromide in carrier materials with complex components. Therefore, it is necessary to develop a new detection method for determining the content of perfluorooctyl bromide in a carrier with DSPC as a pore-forming agent. This method needs to overcome the limitations of the direct injection method of the existing gas chromatography method, be able to adapt to the complexity of the determination of the content of perfluorooctyl bromide in the carrier material, and provide accurate and sensitive analysis results.

[0004] In summary, the development of a new method suitable for the detection of perfluorooctyl bromide content in complex component carriers is of great significance for ensuring product quality and safety, and is also crucial for expanding the application of perfluorooctyl bromide in fields such as medicine. Summary of the invention

[0005] The purpose of the present invention is to provide a method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent, so as to solve the problem that the prior art mainly focuses on directly injecting a test solution and cannot accurately detect the content of perfluorooctyl bromide in a sample with complex components.

[0006] In order to achieve the above object, the present invention provides the following technical solution: a method for detecting perfluorooctane bromide in a carrier using DSPC as a pore-forming agent, comprising:

[0007] S1, firstly pretreating a carrier with DSPC as a pore-forming agent to obtain a sample solution to be tested;

[0008] S2, then prepare the reference solution;

[0009] S3. Analyze and detect the sample solution and the reference solution by gas chromatography, and calculate the content of perfluorooctane bromide in the sample solution.

[0010] Further, the chromatographic conditions of the gas chromatography described in S3 are:

[0011] The chromatographic column is a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid; the injection port temperature is 200℃~240℃; the split ratio is 10:1~20:1; the carrier gas is N2; the flow rate is 0.8ml~1.2ml per minute; the column temperature program is a starting temperature of 30℃, maintained for 7 minutes, and then heated to 180℃ at a rate of 10℃ / min and maintained for 4.5 minutes.

[0012] Furthermore, the preprocessing in S1 includes:

[0013] Weigh 62 mg of a carrier with DSPC as a pore-forming agent, add 5 ml of chloroform to dissolve it, then add 2 ml to 3 ml of water for oscillation extraction, and finally take out the lower chloroform layer, which is the sample solution to be tested.

[0014] Further, the reference solution is then prepared in step S2, comprising:

[0015] Weigh 62 mg of perfluorooctane bromide, place it in a 100 ml volumetric flask, add chloroform solution to dilute to the scale to obtain a control stock solution; measure 1 ml of the control stock solution, place it in a 25 ml volumetric flask, add chloroform solution to dilute to the scale to obtain a control working solution; measure 5 ml of the control working solution, add 2 ml to 3 ml of water for oscillation extraction, and take the lower chloroform layer as the reference solution.

[0016] Furthermore, in S3, the sample solution and the reference solution are analyzed and detected by gas chromatography, and the RSD of the peak area in the chromatogram recorded by the reference solution does not exceed 5.0%.

[0017] Furthermore, the calculation formula of S3 is:

[0018]

[0019] Where: AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested;

[0020] AR is the peak area of ​​perfluorooctane bromide in the reference solution;

[0021] CR is the concentration of the reference solution;

[0022] CI is the concentration of the sample solution to be tested.

[0023] Furthermore, the chromatographic column is DB-624, 30m×0.32mm×1.8μm.

[0024] Furthermore, the detector of the gas chromatography described in S3 is a hydrogen flame ionization detector.

[0025] Furthermore, the temperature of the hydrogen flame ionization detector is 230°C to 270°C.

[0026] Furthermore, the injection volume of the gas chromatography is 1 μl.

[0027] Compared with the prior art, the present invention provides a method for detecting perfluorooctane bromide in a carrier using DSPC as a pore-forming agent. The method is not only simple to operate, but also has high sensitivity and good reproducibility, and can meet the needs of modern analytical chemistry for efficient and accurate detection.

[0028] By selecting a highly sensitive detector and optimizing chromatographic conditions, this method can detect extremely low concentrations of PFOS, which is essential for tracking and monitoring trace changes in PFOS. This feature is particularly important in the fields of environmental monitoring, food safety, and medicine, where trace analysis of PFOS is critical for risk assessment and compliance assurance.

[0029] Through strict experimental design and quality control, the stability and reliability of the method are ensured, and it can provide consistent analytical results at different times, between different operators and different equipment. This not only improves the credibility of the experimental results, but also provides a solid foundation for laboratory management and quality assurance. BRIEF DESCRIPTION OF THE DRAWINGS

[0030] In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments recorded in the present invention. For ordinary technicians in this field, other drawings can also be obtained based on these drawings.

[0031] Figure 1 A schematic diagram of the overall detection method flow provided by an embodiment of the present invention;

[0032] Figure 2 A quantitative limit detection result diagram of the detection method provided in an embodiment of the present invention;

[0033] Figure 3 A graph showing the detection limit detection results of the detection method provided by an embodiment of the present invention;

[0034] Figure 4 A linear curve graph provided for an embodiment of the present invention. DETAILED DESCRIPTION

[0035] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings.

[0036] Embodiment 1:

[0037] See also Figure 1 and Figure 4, a method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent, comprising:

[0038] S1. First, pretreat the carrier with DSPC as the pore-forming agent, weigh 62 mg of the carrier with DSPC as the pore-forming agent, add 5 ml of chloroform to dissolve it, then add 3 ml of water and gently shake and extract, and finally take out the lower chloroform layer, which is the sample solution to be tested, to obtain the sample solution to be tested;

[0039] S2, then prepare the reference solution: weigh 62 mg of perfluorooctane bromide, place it in a 100 ml volumetric flask, add chloroform solution to dilute to the scale, and obtain a reference stock solution; measure 1 ml of the reference stock solution, place it in a 25 ml volumetric flask, add chloroform solution to dilute to the scale, and obtain a reference working solution; measure 5 ml of the reference working solution, add 2 ml to 3 ml of water for oscillation extraction, preferably 3 ml, and take the lower chloroform layer as the reference solution;

[0040] S3. Analyze and detect the sample solution and the reference solution by gas chromatography, and calculate the content of perfluorooctane bromide in the sample solution; in the chromatogram recorded by the reference solution, the RSD of the peak area shall not exceed 5.0%;

[0041] The calculation formula for calculating the content of perfluorooctane bromide in the sample solution and the reference solution is:

[0042]

[0043] Where: AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested;

[0044] AR is the peak area of ​​perfluorooctane bromide in the reference solution;

[0045] CR is the concentration of the reference solution;

[0046] CI is the concentration of the sample solution to be tested;

[0047] The chromatographic conditions of the gas chromatography method are as follows: a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid, model DB-624, 30m×0.32mm×1.8μm; injection port temperature 220℃; split ratio 10:1; carrier gas is N2; flow rate is 1ml / min; column temperature program is a starting temperature of 30℃, maintained for 7 minutes, then heated to 180℃ at a rate of 10℃ / min, maintained for 4.5 minutes; the detector is a hydrogen flame ionization detector, and the detector temperature is 250℃; injection volume 1μl.

[0048] The specific implementation method is as follows: S1, first pre-treat the carrier with DSPC as the pore-forming agent, weigh 62 mg of the carrier with DSPC as the pore-forming agent, add 5 ml of chloroform to dissolve it, then add 3 ml of water and gently shake and extract, and finally take out the lower chloroform layer, which is the sample solution to be tested, to obtain the sample solution to be tested;

[0049] Before weighing the carrier, ensure that the analytical balance is preheated for at least 30 minutes to achieve a stable measurement state. The accuracy of the balance directly affects the quality control of the sample, so the balance needs to be calibrated and maintained regularly.

[0050] Place the carrier in a dry, clean weighing container to avoid contamination by any foreign matter and operate in a stable environment.

[0051] Chloroform can not only effectively dissolve perfluorooctyl bromide, but also maintain the integrity of the carrier material. When using chloroform, attention should be paid to its volatility and potential health risks. Appropriate personal protective equipment should be worn in a well-ventilated environment during operation. When adding chloroform to a carrier with DSPC as a pore-forming agent, it should be poured slowly to avoid excessive foaming. At the same time, it is necessary to ensure that the amount of chloroform is sufficient to completely immerse the carrier to promote the full dissolution of perfluorooctyl bromide, thereby obtaining a mixed solution.

[0052] Then add 3 ml of water to the mixed solution and extract it with slight oscillation. The purpose of oscillation extraction is to ensure that the carrier material (calcium chloride) is fully in contact with water and accelerate the dissolution process of calcium chloride in chloroform. The intensity of oscillation should be moderate to avoid solvent splashing and ensure extraction efficiency. The oscillation time is 1 to 2 minutes to ensure the complete dissolution of calcium chloride in the solution. Too long time may cause unnecessary solvent volatilization or sample decomposition and solution emulsification. The standing time is 1 hour to allow the two layers of liquid to separate completely so that the lower chloroform layer can be clearly identified. The lower chloroform layer separated is the sample solution to be tested.

[0053] When transferring the sample solution to be tested, the time the sample solution is exposed to the air should be minimized to prevent volatilization of the sample. At the same time, splashing or loss of the sample should be avoided to ensure the integrity and representativeness of the sample. Oscillation and standing time can help reduce variability in sample handling and improve the repeatability and reliability of the experiment, which is crucial to ensuring the scientificity and accuracy of the experimental results.

[0054] S2, then prepare the reference solution; weigh 62 mg of perfluorooctane bromide, place it in a 100 ml volumetric flask, add chloroform solution to dilute to the scale, and obtain a reference stock solution; measure 1 ml of the reference stock solution, place it in a 25 ml volumetric flask, add chloroform solution to dilute to the scale, and obtain a reference working solution; measure 5 ml of the reference working solution, add 2 ml to 3 ml of water for oscillation extraction, preferably 3 ml, and take the lower chloroform layer as the reference solution;

[0055] Before weighing perfluorooctyl bromide, make sure that the analytical balance has been calibrated to an accuracy of 0.01 mg to ensure the accuracy of the weighing; the physical state of perfluorooctyl bromide (such as temperature and humidity) will also affect the weighing results, so it should be operated in a controlled environment. When transferring perfluorooctyl bromide from a storage container to a weighing container, special tools such as a syringe should be used to avoid using materials that may react with perfluorooctyl bromide. During the weighing process, the opening time of the weighing container should be minimized to prevent the volatilization or moisture absorption of perfluorooctyl bromide from affecting the weighing results.

[0056] Preparation of reference stock solution: When dissolving perfluorooctane bromide in chloroform, the purity and quality of chloroform should be ensured to avoid the introduction of impurities; the prepared reference stock solution should be clearly labeled with information such as composition, concentration, preparation date and expiration date to ensure traceability.

[0057] The accurate preparation of the control stock solution is the key to the success of the experiment. The concentration of the control stock solution directly affects the accuracy of the reference solution, which in turn affects the results of the entire quantitative analysis. Therefore, the preparation of the control stock solution needs to be carried out strictly in accordance with the standard operating procedures to ensure the accuracy and consistency of the concentration and use it within the validity period.

[0058] Preparation of reference solution: When sampling from the reference stock solution, use an accurate pipette or pipette gun to ensure the accuracy of the sample volume. During the sampling process, avoid contact or contamination to ensure the purity of the reference solution. When adding water for oscillation extraction, pay attention to controlling the intensity and time of oscillation to ensure that the treatment conditions of the reference solution are consistent with those of the sample solution to be tested.

[0059] The purpose of oscillation extraction is to ensure the consistency of the preparation process of the reference solution and the sample processing process. When taking the lower chloroform layer as the reference solution, ensure that the pipetting tool used is clean and dry to avoid contamination. Sampling should be done slowly and carefully to avoid disturbing the liquid surface and causing cross-contamination of the sample. The reference solution transferred to the test tube should be sealed immediately and labeled with the sample information and sampling date. The storage conditions of the reference solution should meet the stability requirements of perfluorooctyl bromide, and it usually needs to be stored away from light and at low temperature.

[0060] The consistency of the preparation process of the reference solution and the sample solution is crucial for the accurate quantification of perfluorooctyl bromide, because any difference in processing may lead to deviations in the analytical results. Various parameters need to be strictly controlled during the preparation of the reference solution to ensure the quality and consistency of the reference solution.

[0061] S3. The sample solution and the reference solution are analyzed and detected by high performance gas chromatography, and the content of perfluorooctane bromide in the sample solution and the reference solution is calculated; a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid is used as the chromatographic column; the injection port temperature is 220°C; the split ratio is 10:1; the carrier gas is N2; the flow rate is 1 ml / min; the column temperature program is a starting temperature of 30°C, maintained for 7 minutes, and then heated to 180°C at a rate of 10°C / min and maintained for 4.5 minutes.

[0062] The chromatographic column is the core of chromatographic analysis. The capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid has unique chemical stability and separation efficiency. This chromatographic column can effectively separate perfluorooctyl bromide and reduce the analysis time.

[0063] The injection port temperature of 220°C is higher than the boiling point of the sample solution to ensure that the sample solution is completely vaporized, which is crucial to avoid clogging of the chromatographic column and ensure effective transmission of the sample solution.

[0064] The split ratio in a gas chromatograph refers to the ratio of the split flow to the column flow. When the split ratio is 10:1, it means that during the split injection process, only 1 / 11 of the sample entering the inlet enters the chromatographic column for separation and analysis, while the remaining 10 / 11 of the sample is diverted and does not enter the chromatographic column. A split ratio of 10:1 helps to improve the separation efficiency of the sample while reducing the load of the sample on the chromatographic column.

[0065] Nitrogen is widely used as a carrier gas due to its chemical stability and low cost. A flow rate of 1 ml / min can achieve the best balance between separation effect and analysis time.

[0066] The column temperature program was as follows: starting at 30 °C, maintaining for 7 min, then increasing to 180 °C at a rate of 10 °C / min and maintaining for 4.5 min. This program was optimized based on the boiling point of perfluorooctane bromide and the characteristics of the chromatographic column.

[0067] The flame ionization detector (FID) has high sensitivity and specific response to perfluorinated compounds. The temperature of the detector is set at 250°C to ensure the best performance of the detector and avoid water vapor condensation.

[0068] Controlling the injection volume is crucial to reducing the dilution effect of the sample and improving detection sensitivity. An injection volume of 1 μl can ensure effective separation of the sample in the chromatographic column while reducing sample waste.

[0069] The sample solution to be tested and the reference solution are analyzed and detected by high performance gas chromatography. In the chromatogram recorded by the reference solution, the RSD of the peak area shall not exceed 5.0%.

[0070] RSD is an important indicator to measure the degree of data dispersion, which can intuitively reflect the degree of discreteness between data. In chromatographic analysis, the smaller the RSD is, the smaller the difference between the data is, and the higher the reliability of the experimental results is. Therefore, limiting RSD to within 5.0% can ensure that the analysis results of the reference solution have high accuracy and repeatability, thereby increasing the reliability of the experimental results.

[0071] The calculation formula for calculating the content of perfluorooctane bromide in the sample solution and the reference solution is:

[0072]

[0073] Content (%) is the value to be calculated, which represents the percentage of perfluorooctane bromide in the sample solution to be tested; AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested. In gas chromatography analysis, the peak area is proportional to the amount of the compound in the sample, so it can be used to measure the amount of perfluorooctane bromide in the sample; AR is the peak area of ​​perfluorooctane bromide in the reference solution. The reference solution is a solution of known concentration, and its peak area can be used to calibrate the instrument to ensure the accuracy of the measurement results; CR is the concentration of the reference solution; CI is the concentration of the sample solution to be tested.

[0074] The calculation process of the formula is as follows: first, the peak area of ​​perfluorooctane bromide in the sample solution (AI) and the reference solution (AR) is obtained by gas chromatography analysis; then, the peak area (AR) and the known concentration (CR) of the reference solution are used to calibrate the instrument to ensure the accuracy of the measurement result; then, the peak area (AI) of the sample solution to be tested is compared with the peak area (AR) of the reference solution to obtain a ratio; finally, this ratio is multiplied by the concentration (CR) of the reference solution, divided by the concentration (CI) of the sample solution to be tested and multiplied by 100% to obtain the percentage of perfluorooctane bromide in the sample solution to be tested.

[0075] Embodiment 2:

[0076] This embodiment provides a technical solution based on the first embodiment: comparison of detection results of different split ratios and injection volumes.

[0077] S1. First, pretreat the carrier with DSPC as the pore-forming agent, weigh 62 mg of the carrier with DSPC as the pore-forming agent, add 5 ml of chloroform to dissolve it, then add 3 ml of water and gently shake and extract, and finally take out the lower chloroform layer, which is the sample solution to be tested, to obtain the sample solution to be tested;

[0078] S2, then prepare the reference solution; weigh 62 mg of perfluorooctane bromide, place it in a 100 ml volumetric flask, add chloroform solution to dilute to the scale, and obtain a reference stock solution; measure 1 ml of the reference stock solution, place it in a 25 ml volumetric flask, add chloroform solution to dilute to the scale, accurately measure 5 ml, add 3 ml of water, shake and extract slightly, and take the chloroform layer as the reference solution;

[0079] S3. Analyze and detect the sample solution and the reference solution by gas chromatography, and calculate the content of perfluorooctane bromide in the sample solution; in the chromatogram recorded by the reference solution, the RSD of the peak area shall not exceed 5.0%;

[0080] The calculation formula for calculating the content of perfluorooctane bromide in the sample solution and the reference solution is:

[0081]

[0082] Where: AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested;

[0083] AR is the peak area of ​​perfluorooctane bromide in the reference solution;

[0084] CR is the concentration of the reference solution;

[0085] CI is the concentration of the sample solution to be tested;

[0086] The chromatographic conditions of the gas chromatography method are as follows: a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid, model DB-624, 30m×0.32mm×1.8μm; injection port temperature 220°C; split ratio 5-20:1; carrier gas is N2; flow rate is 1ml / min; column temperature program is a starting temperature of 30°C, maintained for 7 minutes, then heated to 180°C at a rate of 10°C / min, maintained for 4.5 minutes; the detector is a hydrogen flame ionization detector, and the detector temperature is 250°C; the injection volume is 1μl~2μl.

[0087] The specific test results are as follows:

[0088] Split Ratio Injection volume μl Peak area Tailing Factor Signal-to-Noise Ratio Remark 5:1 2 125.745 0.9 117.5 Poor peak shape, flat peak 10:1 1 41.665 1.2 146.0 good 10:1 2 78.723 0.9 135.6 Slightly flat peak 20:1 1 20.74 1.1 84.2 good

[0089] As mentioned above, when the split ratio was 10:1 and 20:1 and the injection volume was 1 μl, the peak shape was good, the signal-to-noise ratio was high, and the sensitivity was high.

[0090] Embodiment three:

[0091] This embodiment provides a technical solution based on the first embodiment: Comparison of detection results of different extraction volumes:

[0092] A1. First, prepare reference substance stock solution 1#: weigh 62 mg of perfluorooctane bromide, place it in a 50 ml volumetric flask, and dilute to the mark with chloroform solution to obtain reference substance working solution (1); measure 1 ml of reference substance working solution (1), place it in a 50 ml volumetric flask, and dilute to the mark with chloroform solution to obtain reference substance working solution (2); measure 1 ml of reference substance working solution (2), place it in a 10 ml volumetric flask, and dilute to the mark with chloroform solution to obtain reference substance stock solution 1#;

[0093] A2, then pre-treat the carrier with DSPC as the pore-forming agent, weigh 62 mg of the carrier with DSPC as the pore-forming agent, add 0.5 ml of reference substance stock solution 1#, add 4.5 ml of chloroform to dissolve it, then add 2 ml of water and gently shake and extract, finally take out the lower chloroform layer, which is the sample solution to be tested, and obtain the sample solution 1# to be tested;

[0094] A3. Prepare reference substance solution 1#: measure 1 ml of reference substance stock solution 1#, place it in a 10 ml volumetric flask, add chloroform solution to dilute to the mark, and obtain the diluted reference substance stock solution; measure 5 ml of the diluted reference substance stock solution, then add 2 ml of water and gently shake and extract, and finally take out the lower chloroform layer, which is reference substance solution 1#;

[0095] A4, reference stock solution 2#: weigh 62 mg of perfluorooctane bromide, place in a 100 ml volumetric flask, add chloroform solution to dilute to scale to obtain a mother solution; then accurately measure 4 ml of the mother solution, place in a 20 ml volumetric flask, add chloroform solution to dilute to scale to obtain a reference stock solution 2#;

[0096] A5. Test sample solution 2#: Weigh 62 mg of a carrier with DSPC as a pore-forming agent, add 1 ml of the reference stock solution, add 4 ml of chloroform to dissolve it, then add 3 ml of water and shake lightly for extraction, and finally take out the lower chloroform layer, which is the test sample solution 2#.

[0097] A6. Prepare reference solution 2#; weigh 62 mg of perfluorooctane bromide, place in a 100 ml volumetric flask, dilute to scale with chloroform solution to obtain reference stock solution; measure 1 ml of reference stock solution, place in a 25 ml volumetric flask, dilute to scale with chloroform solution, accurately measure 5 ml, add 2 ml to 3 ml of water, shake lightly for extraction, and take the lower chloroform layer, which is reference solution 2#;

[0098] A7. Analyze and detect the sample solution and the reference solution by gas chromatography, and calculate the content of perfluorooctane bromide in the sample solution; the RSD of the peak area in the chromatogram recorded by the reference solution shall not exceed 5.0%;

[0099] The calculation formula for calculating the content of perfluorooctane bromide in the sample solution and the reference solution is:

[0100]

[0101] Where: AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested;

[0102] AR is the peak area of ​​perfluorooctane bromide in the reference solution;

[0103] CR is the concentration of the reference solution;

[0104] CI is the concentration of the sample solution to be tested;

[0105] The chromatographic conditions of the gas chromatography method are as follows: a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid, model DB-624, 30m×0.32mm×1.8μm; injection port temperature 220℃; split ratio 10:1; carrier gas is N2; flow rate is 1ml / min; column temperature program is a starting temperature of 30℃, maintained for 7 minutes, then heated to 180℃ at a rate of 10℃ / min, maintained for 4.5 minutes; the detector is a hydrogen flame ionization detector, and the detector temperature is 250℃; injection volume 1μl.

[0106]

[0107] As mentioned above, when 2 ml and 3 ml of water were added for extraction, the method recovery rate met the requirements.

[0108] Embodiment 4:

[0109] See also Figure 2-Figure 3 This embodiment provides a technical solution based on the first embodiment: the detection limit, sensitivity, reproducibility and accuracy of the detection method are tested.

[0110] The method detection limit (MDL) refers to the lowest concentration or amount that can be detected by the method. This example adopts the signal-to-noise ratio method, that is, by preparing a series of perfluorooctane bromide reference solutions of different concentrations, and measuring them according to the detection method of Example 1, when the signal-to-noise ratio is about 3, the concentration or the amount injected into the instrument is the lowest concentration or amount; when the signal-to-noise ratio is about 10, the concentration or the amount injected into the instrument is the quantitative limit.

[0111] Sensitivity refers to the degree of response of the method to changes in concentration, which is evaluated by the slope of the calibration curve; prepare a series of perfluorooctane bromide reference solutions of known concentrations and measure their response signals; draw a standard curve, that is, a graph of concentration versus response signal, and calculate the slope of the linear regression equation. The larger the slope, the higher the sensitivity.

[0112] Reproducibility refers to the consistency of the results obtained by repeating the experiment under the same conditions. Intra-day reproducibility is to measure the sample solution of the same concentration multiple times (6 times) within one day, and calculate the relative standard deviation (RSD). The smaller the RSD, the better the reproducibility. Inter-day reproducibility is to measure the sample solution of the same concentration multiple times on different days, and also calculate the RSD to evaluate the inter-day reproducibility.

[0113] Accuracy refers to the degree to which the results of the established method are close to the true value or reference value, and is generally expressed as recovery (%). Design 3 different concentrations, prepare at least 3 sample solutions for each concentration for measurement, and use the measurement results of at least 9 samples for evaluation.

[0114] (I) Precision test

[0115] The sample solution was measured by experimenter A according to the detection method of Example 1; and the sample solution was measured by experimenter B according to the detection method of Example 1. After the measurement, the content of perfluorooctane bromide in the 6 test solutions measured by experimenter A and experimenter B was calculated, and the RSD of each and the RSD of the content of the 12 test samples of the two people were calculated.

[0116] Reference stock solution: weigh 62 mg of perfluorooctane bromide, place in a 100 ml volumetric flask, add chloroform solution to dilute to the mark to obtain a mother solution; accurately measure 4 ml of the mother solution, place in a 20 ml volumetric flask to obtain a reference stock solution;

[0117] Sample solution: Weigh 62 mg of a carrier with DSPC as a pore-forming agent, add 1 ml of the reference stock solution and 4 ml of chloroform to dissolve it, then add 3 ml of water and gently shake to extract, and finally take out the lower chloroform layer, which is the sample solution to be tested.

[0118] The specific test results are as follows:

[0119]

[0120]

[0121] As mentioned above, the method has good reproducibility.

[0122] (II) Accuracy test

[0123] The sample solution was measured by the experimenter according to the detection method of Example 1; after the measurement, the recovery rate of the 9 sample solutions was calculated.

[0124] Reference stock solution: weigh 62 mg of perfluorooctane bromide, place in a 100 ml volumetric flask, add chloroform solution to dilute to the mark to obtain a mother solution; accurately measure 4 ml of the mother solution, place in a 20 ml volumetric flask to obtain a reference stock solution;

[0125] Sample solution: Weigh three portions of carrier with DSPC as pore-forming agent, 62 mg each, add 0.5 ml, 1 ml, 1.5 ml of reference stock solution to each portion, then add 4.5 ml, 4 ml, 3.5 ml of chloroform to dissolve, then add 3 ml of water and shake gently for extraction, finally take out the lower chloroform layer, which is the sample solution to be tested. Prepare 3 portions for each concentration. The specific test results are as follows:

[0126]

[0127]

[0128] As mentioned above, the accuracy of this method is good, see Figure 2-Figure 3 The detection limit of this method was 2.4527 ng / μl and the quantification limit was 4.9053 ng / μl.

[0129] The above description is only by way of illustration of certain exemplary embodiments of the present invention. It is undoubted that those skilled in the art can modify the described embodiments in various ways without departing from the spirit and scope of the present invention. Therefore, the above drawings and descriptions are illustrative in nature and should not be construed as limiting the scope of protection of the claims of the present invention.

Claims

1. A method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent, characterized in that: include: S1, firstly pretreating a carrier with DSPC as a pore-forming agent to obtain a sample solution to be tested; S2, then prepare the reference solution; S3. Analyze and detect the sample solution and the reference solution by gas chromatography, and calculate the content of perfluorooctane bromide in the sample solution.

2. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: The chromatographic conditions of the gas chromatography described in S3 are: The chromatographic column is a capillary column with 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary liquid; the injection port temperature is 200℃~240℃; the split ratio is 10:1~20:1; the carrier gas is N2; the flow rate is 0.8ml~1.2ml per minute; the column temperature program is a starting temperature of 30℃, maintained for 7 minutes, and then heated to 180℃ at a rate of 10℃ / min and maintained for 4.5 minutes.

3. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: S1 The preprocessing includes: Weigh 62 mg of the carrier with DSPC as the pore-forming agent, add 5 ml of chloroform to dissolve it, then add 2 ml to 3 ml of water for oscillation extraction, and finally take out the lower chloroform layer, which is the sample solution to be tested.

4. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: Then prepare the reference solution as described in S2, including: Weigh 62 mg of perfluorooctane bromide, place it in a 100 ml volumetric flask, add chloroform solution to dilute to the scale to obtain a control stock solution; measure 1 ml of the control stock solution, place it in a 25 ml volumetric flask, add chloroform solution to dilute to the scale to obtain a control working solution; measure 5 ml of the control working solution, add 2 ml to 3 ml of water for oscillation extraction, and take the lower chloroform layer as the reference solution.

5. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: S3: The sample solution and the reference solution are analyzed and detected by gas chromatography, and the RSD of the peak area in the chromatogram recorded by the reference solution does not exceed 5.0%.

6. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: The calculation formula of S3 is: Where: AI is the peak area of ​​perfluorooctane bromide in the sample solution to be tested; AR is the peak area of ​​perfluorooctane bromide in the reference solution; CR is the concentration of the reference solution; CI is the concentration of the sample solution to be tested.

7. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 2, characterized in that: The chromatographic column is DB-624, 30m×0.32mm×1.8μm.

8. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: The detector of the gas chromatography described in S3 is a hydrogen flame ionization detector.

9. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 8, characterized in that: The temperature of the hydrogen flame ionization detector is 230°C to 270°C.

10. The method for detecting perfluorooctyl bromide in a carrier using DSPC as a pore-forming agent according to claim 1, characterized in that: The injection volume for the gas chromatography was 1 μl.

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