CN112858537A - Rapid detection method for permethrin in anti-mosquito fabric - Google Patents
Rapid detection method for permethrin in anti-mosquito fabric Download PDFInfo
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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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
- G01N30/62—Detectors specially adapted therefor
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
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- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention provides a method for quickly detecting permethrin in an anti-mosquito fabric, which comprises the following steps: (1) crushing a sample to be detected into fragments or powder with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of mixed sample, placing the mixed sample at the bottom of a thermal cracking sample cup, and placing a proper amount of silanized glass wool into the thermal cracking sample cup; (2) preparing a standard product of permethrin; (3) respectively placing the thermal cracking sample cup in the step (1) and the standard substance in the step (2) into thermal cracking equipment, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry combined analysis; (4) and performing qualitative and quantitative detection according to the comparison of the retention time and the peak area of the permethrin in the sample to be detected and the standard substance. The method can accurately and efficiently detect whether the textile contains permethrin or not, the sample does not need to be extracted by a chemical solvent, the detection period is shortened to the maximum extent, the method is environment-friendly and healthy, the sample weighing amount is small, the detection limit is low, and the sensitivity is high.
Description
Technical Field
The invention belongs to the technical field of textile detection, and particularly relates to a rapid detection method for permethrin in an anti-mosquito fabric.
Background
In recent years, different types of anti-mosquito textiles are put on the market and are highly favored by consumers. Permethrin is a pyrethroid insecticide and is a main component of an anti-moth finishing agent widely used in wool spinning industry at present, and although permethrin has the characteristics of broad spectrum and high efficiency, studies show that permethrin has great potential safety hazard, and a mosquito repellent is contacted with skin to generate system side reactions including nerve poisoning, allergy and the like, and the use of high dose can generate adverse effects on special crowds such as children, pregnant women and the like. Standard T/CTCA3-2017 permethrin mosquito-proof fabric of China textile and commerce association group GB18401 the standard specifies the safety evaluation requirement of mosquito-proof fabric and mosquito-proof material, and the content of permethrin in the non-direct contact skin textile is less than 1g/m2The content of permethrin in the textile directly contacted with the skin is less than 0.8g/m2The content of permethrin in the textile for children is less than 0.2g/m2The permethrin in the textiles is determined by the national standard GB/T18412.4-2006 part 4 of determination of pesticide residue on textiles: pyrethroid pesticide, 80mL of acetone-n-hexane mixed solvent is adopted for extraction in pretreatment, 5mL of n-hexane is used for constant volume after spinning drying, a lot of solvent and time are consumed, and the use of an organic solvent has certain harm to the environment.
Considering that the detection rate of permethrin in textiles is relatively low in actual detection, an accurate and efficient permethrin rapid detection method is very necessary to be established for accelerating the detection speed, shortening the detection period and reducing or even avoiding the use of organic reagents.
Disclosure of Invention
Aiming at the problems of long pretreatment time, adoption of an organic reagent as an extraction solvent, complex process and the like of the existing detection method, the invention provides the rapid detection method for permethrin in the textile, samples do not need to be pretreated, analysis can be carried out after weighing, and the problem of recontamination of an organic solvent does not exist.
In order to achieve the purpose, the invention adopts the following technical scheme:
a rapid detection method for permethrin in an anti-mosquito fabric utilizes a thermal cracking-gas chromatography-mass spectrometer to detect permethrin, and comprises the following steps:
(1) crushing a sample to be tested into fragments or powder with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of mixed sample, placing the mixed sample at the bottom of a thermal cracking sample cup, placing a proper amount of silanized glass wool into the thermal cracking sample cup, and covering the sample to prevent the sample from floating;
(2) preparing a standard product of permethrin;
(3) respectively placing the thermal cracking sample cup in the step (1) and the standard substance in the step (2) into thermal cracking equipment, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry combined analysis;
(4) and performing qualitative and quantitative detection according to the comparison of the retention time and the peak area of the permethrin in the sample to be detected and the standard substance.
The invention is further set that the weight of the weighed sample to be measured is 0.50-1.50 mg, and the accuracy is 0.01 mg.
The invention is further configured that the thermal cracking conditions are: and (3) heating by adopting a micro-furnace type, wherein the thermal cracking temperature is 400-600 ℃, and the thermal cracking time is 20-90 s.
The invention is further configured that the preparation method of the standard permethrin comprises the following steps: and (3) absorbing the standard working solution of the permethrin, injecting the solution into a thermal cracking sample cup, and volatilizing the solvent to obtain the permethrin standard product.
The invention is further configured that the preparation method of the standard working solution comprises the following steps: quantitatively weighing a standard substance of permethrin, dissolving the standard substance in an organic solvent, and preparing into a standard stock solution; and diluting the standard stock solution into standard working solutions with different gradients.
The invention is further configured such that the organic solvent is n-hexane.
The invention is further set that the working conditions of the gas chromatography-tandem mass spectrometry combined analysis are as follows: the chromatographic column is DB-5MS, 30.0 mm × 0.25 μm or other similar capillary columns; the carrier gas is high-purity helium; the flow rate of the column is 1.0-1.5 mL/min; the temperature of a sample inlet is 250-300 ℃; split-flow sample injection, wherein the split-flow ratio is (10-130): 1; temperature programming: the initial temperature is 40-80 ℃, the temperature is kept for 0-5 min, the temperature is raised to 150 ℃ at the speed of 10-50 ℃/min, the temperature is raised to 280-330 ℃ at the speed of 20-60 ℃/min, and the temperature is kept for 5-10 min.
The invention is further set that the working conditions of the mass spectrum of the gas chromatography-tandem mass spectrometry are as follows: adopting an EI ion source: 70eV, the temperature of an ion source is 230-300 ℃, the temperature of a gas-mass interface is 270-320 ℃, Q2 collision gas is high-purity argon, a mass spectrum scanning Selective Reaction Monitoring (SRM) mode is adopted, and parameters of monitoring ions and collision voltage of a tandem mass spectrum are shown in the following table:
the invention is further set up in that the qualitative and quantitative analysis method of permethrin is as follows: after gas chromatography-mass spectrometry combined analysis, comparing the retention time of the chromatographic peak of the mass of the sample to be detected with that of the standard mass, if the retention time of the chromatographic peak of the mass of permethrin in the sample to be detected is consistent with that of the corresponding standard substance, the allowable deviation is less than +/-2.5%; and the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the following table, the existence of the corresponding permethrin in the sample to be detected can be judged.
| Relative ion abundance | ＞50％ | More than 20 percent and less than or equal to 50 percent | More than 10 percent and less than or equal to 20 percent | ≤10％ |
| Allowable relative deviation | ±20％ | ±25％ | ±30％ | ±50％ |
The invention is further arranged that the content of permethrin in the sample to be tested is calculated according to the following formula:
X＝Ai×Cis/(Ais×m) (1)
wherein: x is the content of permethrin in the sample, and the unit is microgram per gram (mu g/g);
Aithe response peak area of permethrin in the sample to be detected is shown;
Cisthe absolute mass of permethrin in the standard substance is nanogram (ng);
Aisthe area of the response peak of permethrin in the standard substance is shown;
m is the sample weight in milligrams (mg).
The invention has the beneficial effects that:
compared with the prior art, the method for rapidly detecting permethrin in the textile has the advantages that the sample does not need chemical solvent extraction pretreatment, and the detection is simpler; no organic solvent recontamination exists, so that the environment is protected and the health is improved; the method can be used for qualitatively and quantitatively detecting the permethrin by combining a trace analysis technology of gas chromatography-tandem mass spectrometry, and has the detection limit of 0.05mg/kg, low detection limit and high sensitivity.
The method shortens the detection period to the maximum extent, can promote the green sustainable development of the textile industry chain to a certain extent, improves the product quality of the textile industry in China, and provides necessary technical support for enhancing the quality monitoring of the ecological safety of textiles.
Drawings
FIG. 1 is a selective ion chromatogram of permethrin standard with an absolute mass of 10 ng;
FIG. 2 is a selected ion chromatogram of a test sample in example 1;
FIG. 3 is a selected ion chromatogram of a test sample to be tested according to example 2;
FIG. 4 is a selected ion chromatogram of a test sample to be tested according to example 3;
FIG. 5 is a selected ion chromatogram of a sample to be tested in example 4.
Detailed Description
The present invention will be described in further detail with reference to examples. It is to be understood that the following examples are for illustrative purposes only and are not to be construed as limiting the scope of the present invention, and that certain insubstantial modifications and adaptations of the invention may be made by those skilled in the art based on the teachings herein.
Example 1
Detecting permethrin in a textile sample with 100% lyocell textile fibre composition:
(1) taking a textile sample of blue-white alternate stripes and 100% lyocell, shearing the textile sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 0.50mg of mixed sample, and placing the mixed sample at the bottom of a thermal cracking sample cup; putting a proper amount of silanized glass wool into the thermal cracking sample cup for covering the sample to prevent the sample from floating out;
(2) adopting n-hexane mixture as a solvent, weighing a standard substance of permethrin, preparing a standard stock solution with the concentration of 1000 +/-50 mu g/mL, and diluting the standard stock solution into standard working solutions with the concentrations of 100 mu g/mL, 10 mu g/mL and 1 mu g/mL step by step; respectively transferring 5 mu L of 1 mu g/mL standard working solution, 1 mu L of 10 mu g/mL standard working solution, 2 mu L of 4 mu L of 8 mu L of 10 mu g/mL standard working solution and 10 mu L of 100 mu g/mL standard working solution into a thermal cracking sample cup, volatilizing the solvent, and respectively setting the absolute contents of permethrin in the thermal cracking sample cup as follows: 5ng, 10ng, 20ng, 40ng, 80ng, 100ng, 1000 ng;
(3) putting the thermal cracking sample cup in the steps (1) and (2) into thermal cracking equipment combining thermal cracking-gas chromatography-tandem mass spectrometry, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry, wherein:
the thermal cracking adopts micro-furnace heating, the thermal cracking temperature is 400 ℃, and the thermal cracking time is 90 s;
the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is helium; the column flow rate is 1.3 mL/min; the temperature of a sample inlet is 270 ℃; split-flow sample injection, the split-flow ratio is 20: 1; temperature programming: the initial temperature is 60 ℃, the temperature is kept for 1min, the temperature is increased to 150 ℃ at the speed of 15 ℃/min, and the temperature is increased to 280 ℃ at the speed of 50 ℃/min and kept for 6 min.
The mass spectrum adopts an EI ion source: 70eV, 250 ℃ of the ion source, 270 ℃ of the gas mass interface, and a reaction monitoring (SRM) mode, wherein the parameters of the monitoring ions and the collision voltage of the optimized tandem mass spectrum are shown in the summary of the invention.
FIG. 1 is a selective ion chromatogram of a standard substance with an absolute content of 10ng, wherein the retention time of the appearance peaks of permethrin I and permethrin II in the chromatogram is respectively 13.80min and 13.89min, the peaks can be separated from each other, and the peaks are sharp and have good symmetry; the selected monitoring ions have high sensitivity, good selectivity, less interference, wide linear range, accurate qualitative determination and low quantitative limit.
The selective monitoring ion chromatogram of the sample to be detected is shown in figure 2, the sample to be detected and the standard product have permethrin I and permethrin II peaks at the same retention time of 13.81min and 13.91min, and the deviation is less than +/-2.5%; the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the invention content, and the existence of the corresponding permethrin in the sample to be detected can be judged.
Fitting a linear equation according to the relation between the peak areas and the absolute contents of the standard substances with different gradients: 44835x (y is peak area, x is content, unit is ng), and the content of permethrin in 0.5mg of the textile sample is calculated according to the formula (1): 28ng, namely the content of permethrin in the sample to be detected is 56 mug/g.
Example 2
Detecting permethrin in a textile sample with 9.98 percent of spandex and 90.02 percent of chinlon as textile fiber components:
(1) taking a textile sample which is white-background red and contains 9.98% of spandex and 90.02% of chinlon, shearing the textile sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 1.00mg of mixed sample, and placing the mixed sample at the bottom of a thermal cracking sample cup; putting a proper amount of silanized glass wool into the thermal cracking sample cup for covering the sample to prevent the sample from floating out;
(2) preparing a standard permethrin, which is the same as the step (2) in the example 1;
(3) putting the thermal cracking sample cup in the steps (1) and (2) into thermal cracking equipment combining thermal cracking-gas chromatography-tandem mass spectrometry, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry, wherein:
the thermal cracking adopts micro-furnace heating, the thermal cracking temperature is 450 ℃, and the thermal cracking time is 60 s;
the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is helium; the column flow rate is 1.0 mL/min; the temperature of a sample inlet is 250 ℃; split-flow sample injection, the split-flow ratio is 100: 1; temperature programming: the initial temperature is 40 ℃, the temperature is kept for 3min, the temperature is raised to 150 ℃ at the speed of 20 ℃/min, and the temperature is raised to 300 ℃ at the speed of 60 ℃/min and kept for 5 min.
The mass spectrum adopts an EI ion source: 70eV, 260 ℃ of the ion source, 300 ℃ of the gas mass interface, and a reaction monitoring (SRM) mode is selected, and the parameters of the monitoring ions and the collision voltage of the optimized tandem mass spectrum are shown in the invention.
The selection ion chromatogram of the standard substance is shown in figure 1, the selection monitoring ion chromatogram of the sample to be tested is shown in figure 3, the sample to be tested and the standard substance have permethrin I and permethrin II peaks at the same retention time of 13.83min and 13.92min, and the deviation is less than +/-2.5%; the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the invention content, and the existence of the corresponding permethrin in the sample to be detected can be judged.
Fitting a linear equation according to the relation between the peak areas and the absolute contents of the standard substances with different gradients: 44798x (y is peak area, x is content, unit is ng), calculated according to formula (1) to give 1.00mg of textile sample with permethrin content: 526ng, namely the content of the permethrin in the sample to be detected is 526 mug/g.
Example 3
Detecting permethrin in a textile sample with a textile fiber component of 100% of nylon:
(1) selecting a blue textile sample with 100% of chinlon, shearing the textile sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 1.50mg of a mixed sample, and placing the mixed sample at the bottom of a thermal cracking sample cup; putting a proper amount of silanized glass wool into the thermal cracking sample cup for covering the sample to prevent the sample from floating out;
(2) preparing a standard permethrin, which is the same as the step (2) in the example 1;
(3) putting the thermal cracking sample cup in the steps (1) and (2) into thermal cracking equipment combining thermal cracking-gas chromatography-tandem mass spectrometry, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry, wherein:
the thermal cracking adopts micro-furnace heating, the thermal cracking temperature is 500 ℃, and the thermal cracking time is 40 s;
the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is helium; the column flow rate is 1.5 mL/min; the temperature of a sample inlet is 300 ℃; split-flow sample injection, the split-flow ratio is 50: 1; temperature programming: the initial temperature is 50 ℃, the temperature is kept for 2min, the temperature is increased to 150 ℃ at the speed of 30 ℃/min, and the temperature is increased to 290 ℃ at the speed of 40 ℃/min, and the temperature is kept for 8 min.
The mass spectrum adopts an EI ion source: 70eV, 280 ℃ of the ion source, 280 ℃ of the gas-mass interface, and selecting a reaction monitoring (SRM) mode, wherein the optimized parameters of the monitoring ions and the collision voltage of the tandem mass spectrum are shown in the summary of the invention.
The selection ion chromatogram of the standard substance is shown in figure 1, the selection monitoring ion chromatogram of the sample to be tested is shown in figure 4, the sample to be tested and the standard substance have permethrin I and permethrin II peaks at the same retention time of 13.80min and 13.91min, and the deviation is less than +/-2.5%; the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the invention content, and the existence of the corresponding permethrin in the sample to be detected can be judged.
Fitting a linear equation according to the relation between the peak areas and the absolute contents of the standard substances with different gradients: y 44878x (y is peak area, x is content, unit is ng), and the content of permethrin in 1.50mg of textile sample is calculated according to formula (1): 2063ng, namely the content of permethrin in the sample to be detected is 1375 mug/g.
Example 4
Detection of permethrin in a textile sample with 100% polyester textile fibre composition:
(1) selecting a textile sample with flower color and 100% polyester as components, shearing the textile sample into fragments or powder with the particle size of less than 0.5mm by using scissors, uniformly mixing, weighing 0.80mg of mixed sample, and placing the mixed sample at the bottom of a thermal cracking sample cup; putting a proper amount of silanized glass wool into the thermal cracking sample cup for covering the sample to prevent the sample from floating out;
(2) preparing a standard permethrin, which is the same as the step (2) in the example 1;
(3) putting the thermal cracking sample cup in the steps (1) and (2) into thermal cracking equipment combining thermal cracking-gas chromatography-tandem mass spectrometry, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry, wherein:
the thermal cracking adopts micro-furnace heating, the thermal cracking temperature is 600 ℃, and the thermal cracking time is 20 s;
the chromatographic column is DB-5MS, 30.0 mm multiplied by 0.25 mu m; the carrier gas is helium; the column flow rate is 1.2 mL/min; the injection port temperature is 290 ℃; split-flow sample injection, wherein the split-flow ratio is 130: 1; temperature programming: the initial temperature is 80 ℃, the temperature is kept for 5min, the temperature is increased to 150 ℃ at the speed of 50 ℃/min, and the temperature is increased to 330 ℃ at the speed of 50 ℃/min and kept for 6 min.
The mass spectrum adopts an EI ion source: 70eV, 300 ℃ of the ion source, 320 ℃ of the gas mass interface, and a reaction monitoring (SRM) mode, wherein the parameters of the monitoring ions and the collision voltage of the optimized tandem mass spectrum are shown in the summary of the invention.
The selection ion chromatogram of the standard substance is shown in figure 1, the selection monitoring ion chromatogram of the sample to be tested is shown in figure 5, the sample to be tested and the standard substance have permethrin I and permethrin II peaks at the same retention time of 13.87min and 13.94min, and the deviation is less than +/-2.5%; the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the invention content, and the existence of the corresponding permethrin in the sample to be detected can be judged.
Fitting a linear equation according to the relation between the peak areas and the absolute contents of the standard substances with different gradients: 44665x (y is the peak area, x is the content, in ng), and the permethrin content in 0.80mg of textile sample was calculated according to equation (1) as: 1346ng, namely the content of the permethrin in the sample to be detected is 1682 mug/g.
Claims (10)
1. A rapid detection method for permethrin in an anti-mosquito fabric is characterized in that the permethrin is detected by using a thermal cracking-gas chromatography-mass spectrometer, and the method comprises the following steps:
(1) crushing a sample to be tested into fragments or powder with the particle size of less than 0.5mm, uniformly mixing, weighing a proper amount of mixed sample, placing the mixed sample at the bottom of a thermal cracking sample cup, placing a proper amount of silanized glass wool into the thermal cracking sample cup, and covering the sample to prevent the sample from floating;
(2) preparing a standard product of permethrin;
(3) respectively placing the thermal cracking sample cup in the step (1) and the standard substance in the step (2) into thermal cracking equipment, and carrying out thermal cracking-gas chromatography-tandem mass spectrometry combined analysis;
(4) and performing qualitative and quantitative detection according to the comparison of the retention time and the peak area of the permethrin in the sample to be detected and the standard substance.
2. The detection method according to claim 1, wherein the weighed sample to be detected has a mass of 0.50-1.50 mg, and is accurate to 0.01 mg.
3. The detection method according to claim 1, wherein the thermal cracking conditions are: and (3) heating by adopting a micro-furnace type, wherein the thermal cracking temperature is 400-600 ℃, and the thermal cracking time is 20-90 s.
4. The detection method as claimed in claim 1, wherein the standard substance of permethrin is prepared by the following steps: and (3) absorbing the standard working solution of the permethrin, injecting the solution into a thermal cracking sample cup, and volatilizing the solvent to obtain the permethrin standard product.
5. The detection method according to claim 4, wherein the standard working solution is prepared by: quantitatively weighing a standard substance of permethrin, dissolving the standard substance in an organic solvent, and preparing into a standard stock solution; and diluting the standard stock solution into standard working solutions with different gradients.
6. The detection method according to claim 5, wherein the organic solvent is n-hexane.
7. The detection method according to claim 1, wherein the working conditions of the gas chromatography-tandem mass spectrometry are as follows: the chromatographic column is DB-5MS, 30.0 mm × 0.25 μm or other similar capillary columns; the carrier gas is high-purity helium; the flow rate of the column is 1.0-1.5 mL/min; the temperature of a sample inlet is 250-300 ℃; split-flow sample injection, wherein the split-flow ratio is (10-130): 1; temperature programming: the initial temperature is 40-80 ℃, the temperature is kept for 0-5 min, the temperature is raised to 150 ℃ at the speed of 10-50 ℃/min, the temperature is raised to 280-330 ℃ at the speed of 20-60 ℃/min, and the temperature is kept for 5-10 min.
8. The detection method according to claim 1, wherein the working conditions of the mass spectrum of the GC-MS are as follows: adopting an EI ion source: 70eV, the temperature of an ion source is 230-300 ℃, the temperature of a gas-mass interface is 270-320 ℃, Q2 collision gas is high-purity argon, a mass spectrum scanning Selective Reaction Monitoring (SRM) mode is adopted, and parameters of monitoring ions and collision voltage of a tandem mass spectrum are shown in the following table.
9. The detection method as claimed in claim 1, wherein the qualitative and quantitative analysis method of permethrin is as follows: after gas chromatography-tandem mass spectrometry combined analysis, comparing the retention time of the chromatographic peak of the mass of the sample to be detected with that of the standard mass, if the retention time of the chromatographic peak of the mass of permethrin in the sample to be detected is consistent with that of the corresponding standard substance, the allowable deviation is less than +/-2.5%; and the relative deviation between the relative ion abundance of the qualitative ion pair and the relative ion abundance of the standard substance with the equivalent concentration does not exceed the range shown in the following table, judging that the corresponding permethrin exists in the sample to be detected.
10. The detection method according to claim 1, wherein the content of permethrin in the sample to be detected is calculated according to the following formula:
X＝Ai×Cis/(Ais×m) (1)
wherein: x is the content of permethrin in the sample, and the unit is microgram per gram (mu g/g);
Aithe response peak area of permethrin in the sample to be detected is shown;
Cisthe absolute mass of permethrin in the standard substance is nanogram (ng);
Aisthe area of the response peak of permethrin in the standard substance is shown;
m is the sample weight in milligrams (mg).
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| CN114460200A (en) * | 2022-02-09 | 2022-05-10 | 上海市质量监督检验技术研究院 | Method for identifying silk cotton methacrylamide grafting weight gain |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0843374A (en) * | 1994-07-26 | 1996-02-16 | Shimadzu Corp | Chromatographic mass-spectrography device using sim method |
| US20050132500A1 (en) * | 2003-12-22 | 2005-06-23 | Basf Aktiengesellschaft | Composition for impregnation of fibers, fabrics and nettings imparting a protective activity against pests |
| BRPI0800544A2 (en) * | 2008-02-01 | 2009-12-08 | Macedo Rui Oliveira | Analytical technology based on pyrolysis coupled to gas chromatography / mass spectrometry to characterize and obtain chemical compounds from nebulized dry passiflora alata curtis extracts |
| CN103293267A (en) * | 2013-06-08 | 2013-09-11 | 国家烟草质量监督检验中心 | GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product |
| CN103675081A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for quickly and sensitively detecting pesticide residues on surfaces of fruits and vegetables |
| CN105067748A (en) * | 2015-08-07 | 2015-11-18 | 通标标准技术服务(上海)有限公司 | Method used for determining melamine resin in textiles |
| CN107085047A (en) * | 2017-04-07 | 2017-08-22 | 浙江工业大学 | The analysis method of polyacrylic acid and its esters polymer in a kind of detection textile |
| CN107290449A (en) * | 2017-06-15 | 2017-10-24 | 深圳职业技术学院 | Three in a kind of textile（2 chloroethyls）The quick selective mechanisms method of phosphate |
| CN108535474A (en) * | 2018-03-16 | 2018-09-14 | 北方工业大学 | Time-resolved fluorescence test strip for detecting permethrin and application thereof |
| DE102017010791A1 (en) * | 2017-11-22 | 2019-05-23 | Bundesrepublik Deutschland, vertreten durch das Bundesministerium der Verteidigung, vertreten durch das Bundesamt für Ausrüstung, Informationstechnik und Nutzung der Bundeswehr | Textile product with permethrin as vector protection |
| CN109975468A (en) * | 2019-02-15 | 2019-07-05 | 上海市质量监督检验技术研究院 | The detection method of mosquito repellent effective component in a kind of textile |
-
2021
- 2021-04-14 CN CN202110400506.1A patent/CN112858537B/en active Active
Patent Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0843374A (en) * | 1994-07-26 | 1996-02-16 | Shimadzu Corp | Chromatographic mass-spectrography device using sim method |
| US20050132500A1 (en) * | 2003-12-22 | 2005-06-23 | Basf Aktiengesellschaft | Composition for impregnation of fibers, fabrics and nettings imparting a protective activity against pests |
| BRPI0800544A2 (en) * | 2008-02-01 | 2009-12-08 | Macedo Rui Oliveira | Analytical technology based on pyrolysis coupled to gas chromatography / mass spectrometry to characterize and obtain chemical compounds from nebulized dry passiflora alata curtis extracts |
| CN103675081A (en) * | 2012-09-13 | 2014-03-26 | 中国科学院大连化学物理研究所 | Method for quickly and sensitively detecting pesticide residues on surfaces of fruits and vegetables |
| CN103293267A (en) * | 2013-06-08 | 2013-09-11 | 国家烟草质量监督检验中心 | GC-MS/MS (gas chromatography-tandem mass spectrometry) method for analyzing pyrethroid pesticide residue in tobacco and tobacco product |
| CN105067748A (en) * | 2015-08-07 | 2015-11-18 | 通标标准技术服务(上海)有限公司 | Method used for determining melamine resin in textiles |
| CN107085047A (en) * | 2017-04-07 | 2017-08-22 | 浙江工业大学 | The analysis method of polyacrylic acid and its esters polymer in a kind of detection textile |
| CN107290449A (en) * | 2017-06-15 | 2017-10-24 | 深圳职业技术学院 | Three in a kind of textile（2 chloroethyls）The quick selective mechanisms method of phosphate |
| DE102017010791A1 (en) * | 2017-11-22 | 2019-05-23 | Bundesrepublik Deutschland, vertreten durch das Bundesministerium der Verteidigung, vertreten durch das Bundesamt für Ausrüstung, Informationstechnik und Nutzung der Bundeswehr | Textile product with permethrin as vector protection |
| CN108535474A (en) * | 2018-03-16 | 2018-09-14 | 北方工业大学 | Time-resolved fluorescence test strip for detecting permethrin and application thereof |
| CN109975468A (en) * | 2019-02-15 | 2019-07-05 | 上海市质量监督检验技术研究院 | The detection method of mosquito repellent effective component in a kind of textile |
Non-Patent Citations (9)
| Title |
|---|
| ELENA PERDUM: "An analytical approach for extraction and detection of permethrin from functionalized textile materials", INDUSTRIA TEXTILA, vol. 70, no. 2 * |
| JUDITH B SENNETT: "A New Method for Determining Permethrin Level on Military Uniform Fabrics", 《US ARMY RESEARCH LABORATORY》 * |
| JUDITH B SENNETT: "A New Method for Determining Permethrin Level on Military Uniform Fabrics", 《US ARMY RESEARCH LABORATORY》, 30 June 2017 (2017-06-30), pages 2 - 5 * |
| 刘彩明: "Py-GC-MS快速测定纺织品中12种高关注物质", 《针织工业》 * |
| 刘彩明: "Py-GC-MS快速测定纺织品中12种高关注物质", 《针织工业》, no. 9, 30 September 2020 (2020-09-30), pages 68 - 72 * |
| 吴胜芳;王利平;刘杨岷;虞锐鹏;: "加速溶剂萃取-气相色谱串联质谱测定菊花中的3种菊酯类农药残留量", 分析试验室, no. 11 * |
| 张焱: "棉纺织品中7种残留拟除虫菊酯杀虫剂的检测", 《北京服装学院学报(自然科学版)》 * |
| 张焱: "棉纺织品中7种残留拟除虫菊酯杀虫剂的检测", 《北京服装学院学报(自然科学版)》, vol. 30, no. 4, 31 October 2010 (2010-10-31), pages 55 - 62 * |
| 范志先;赵文英;贾淑敏;王树娟;傅慧;: "反相高效液相色谱法测定纺织品上的氯菊酯", 青岛科技大学学报(自然科学版), no. 04 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114460200A (en) * | 2022-02-09 | 2022-05-10 | 上海市质量监督检验技术研究院 | Method for identifying silk cotton methacrylamide grafting weight gain |
| CN114460200B (en) * | 2022-02-09 | 2023-08-08 | 上海市质量监督检验技术研究院 | Method for identifying weight gain of silk floss methacrylamide grafted polymer |
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