CN113933425B - Method for measuring content of acetophenone azine in plastic, chloroprene rubber or foam - Google Patents
Method for measuring content of acetophenone azine in plastic, chloroprene rubber or foam Download PDFInfo
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- CN113933425B CN113933425B CN202111188863.2A CN202111188863A CN113933425B CN 113933425 B CN113933425 B CN 113933425B CN 202111188863 A CN202111188863 A CN 202111188863A CN 113933425 B CN113933425 B CN 113933425B
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- 239000006260 foam Substances 0.000 title claims abstract description 33
- 229920001084 poly(chloroprene) Polymers 0.000 title claims abstract description 29
- 229920003023 plastic Polymers 0.000 title claims abstract description 26
- 239000004033 plastic Substances 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 24
- MOKMQSIJAHPSQX-JTFWXBGUSA-N (z)-1-phenyl-n-[(z)-1-phenylethylideneamino]ethanimine Chemical compound C=1C=CC=CC=1C(/C)=N\N=C(\C)C1=CC=CC=C1 MOKMQSIJAHPSQX-JTFWXBGUSA-N 0.000 title claims abstract description 11
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims abstract description 96
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims abstract description 45
- 238000000605 extraction Methods 0.000 claims abstract description 31
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 claims abstract description 20
- 238000002156 mixing Methods 0.000 claims abstract description 14
- 238000007789 sealing Methods 0.000 claims abstract description 12
- 238000005259 measurement Methods 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 9
- 238000001819 mass spectrum Methods 0.000 claims abstract description 5
- 238000011049 filling Methods 0.000 claims abstract description 3
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 30
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 238000001514 detection method Methods 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 238000011088 calibration curve Methods 0.000 claims description 4
- 238000010812 external standard method Methods 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 3
- 239000012159 carrier gas Substances 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000011002 quantification Methods 0.000 claims 1
- 238000002390 rotary evaporation Methods 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000002137 ultrasound extraction Methods 0.000 abstract description 6
- 238000001914 filtration Methods 0.000 abstract description 3
- 238000004949 mass spectrometry Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 238000010298 pulverizing process Methods 0.000 description 3
- 239000005060 rubber Substances 0.000 description 3
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 2
- 239000013566 allergen Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- 206010012442 Dermatitis contact Diseases 0.000 description 1
- 206010020751 Hypersensitivity Diseases 0.000 description 1
- RFFFKMOABOFIDF-UHFFFAOYSA-N Pentanenitrile Chemical compound CCCCC#N RFFFKMOABOFIDF-UHFFFAOYSA-N 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 208000010247 contact dermatitis Diseases 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229960005489 paracetamol Drugs 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000003206 sterilizing agent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- 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
- G01N2030/042—Standards
- G01N2030/047—Standards external
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a method for measuring the content of acetophenone azine in plastics, neoprene and foam, which comprises the following steps: 1) Cutting the sample, uniformly mixing the cut sample, filling the mixture into a self-sealing bag, and sealing and preserving the mixture for later use; accurately weighing a proper amount of sample in a centrifuge tube after uniformly mixing; 2) Adding n-hexane into a plastic sample or a chloroprene rubber sample for ultrasonic extraction; transferring the foam sample into a needle tube with a needle removed, and adding n-hexane for ultrasonic extraction; then, the extract is distilled to near dryness, acetonitrile is used for constant volume, and a gas chromatograph with mass spectrum is used for measurement after filtration; 3) Determining the concentration of the acetophenone in the sample extraction solution by a GC-MS method; 4) Calculating the content of the acetophenone in the sample according to the concentration of the acetophenone in the sample extraction solution; the invention has the advantages of quick and simple measurement, and can realize the accurate measurement of the content of the acetophenone azine in plastics, neoprene and foam, and the minimum quantitative concentration is 2mg/kg.
Description
[ Technical field ]
The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for measuring the content of acetophenone azine in plastics, chloroprene rubber or foam.
[ Background Art ]
The acetophenone azine is a white powder compound with the relative density of 0.98g/cm 3 (22 ℃), the melting point of 121-122 ℃ and the boiling point of 333.2 ℃ (decomposition) and is prepared by reacting hydrazine hydrate with acetophenone, and is often used as a sterilizing agent in plastic, chloroprene rubber and foam. It has been previously reported that allergic reactions often appear as contact dermatitis in some sensitive people in the long-term or repeated exposure to acetophenone environments, whereas allergens are usually some of the rubber components, dyes, benzoyl peroxide or formaldehyde resins, mainly through the irritating reactions caused by friction and perspiration of the human body after contact with the latter. Patch tests combined with ultrasonic water bath extraction demonstrated that acetophenone was one of the allergens. The synthesis raw material of the acetophenone is acetophenone, and the acetophenone and the impurity synthesis raw material of the acetophenone, the dicumyl peroxide are all sensitized. While no regulations currently exist for the management of acetaminophen, some buyers have required that the content of plastic, rubber or foam filler supplied by suppliers be no more than 50mg/kg.
Aiming at the fact that no detection method for the content of the acetophenone in plastics, neoprene and foam exists in China at present, the establishment of a detection method for the content of the acetophenone in plastics, neoprene and foam is urgent.
[ Summary of the invention ]
The invention aims to solve the defects and provide a method for measuring the content of the acetophenone in plastics, neoprene and foam, which is quick and simple, can accurately measure the content of the acetophenone in plastics, neoprene and foam, and has the lowest quantitative concentration of 2mg/kg.
In order to achieve the above purpose, a method for measuring the content of acetophenone azine in plastics, neoprene and foam is designed, which comprises the following steps:
1) Sample pretreatment: cutting the sample with scissors or pulverizing with pulverizer, mixing the pulverized sample uniformly, and packaging into clean and dry self-sealing bag, sealing and preserving for use; accurately weighing a proper amount of sample in a centrifuge tube after uniformly mixing; the sample is a plastic sample, a chloroprene rubber sample or a foam sample;
2) Extraction of the sample: firstly, adding n-hexane into a plastic sample or a chloroprene rubber sample for ultrasonic extraction; transferring the foam sample into a needle tube with a needle removed, and adding n-hexane for ultrasonic extraction; then, the extract is distilled to near dryness, acetonitrile is used for constant volume, and a gas chromatograph with mass spectrum is used for measurement after filtration;
3) Determining the concentration of the acetophenone in the sample extraction solution obtained in the step 2) by adopting a GC-MS gas chromatography-mass spectrometry method;
4) Calculating the content of the acetophenone in the sample according to the concentration of the acetophenone in the sample extraction solution obtained in the step 3).
Preferably, in step 1), the sample is sheared with scissors or crushed into 2X 2mm pieces with a crusher; after mixing, 0.50 g.+ -. 0.01g of sample is weighed accurately into a 50mL centrifuge tube.
Preferably, in the step 2), 5mL of normal hexane is added into a plastic sample or a chloroprene rubber sample for extraction, the extraction liquid is completely transferred to a 50mL flat-bottomed flask after being subjected to ultrasonic treatment at room temperature for 30min, a centrifuge tube is washed by using 5mL of normal hexane, the solutions are combined into the flat-bottomed flask, the solution is steamed until the solution is nearly dry by rotating, and 1mL of acetonitrile is used for fixing the volume; the acetonitrile solution was then transferred to a sample vial after passing through a 0.45 μm organic filter head and measured using a gas chromatograph equipped with mass spectrometry.
Preferably, in the step 2), the foam sample is added with 15mL of normal hexane for extraction, the extraction liquid is completely transferred to a 50mL flat-bottomed flask after ultrasonic treatment is carried out for 30min at room temperature, the sample is transferred to a needle tube with a needle removed, the sample is extruded by a push rod, and the extraction liquid absorbed by the sample is extruded into the flat-bottomed flask as much as possible; the centrifuge tube is washed by 5mL of normal hexane, the solution is combined into a flat-bottomed flask, the mixture is steamed to be nearly dry, and 1mL of acetonitrile is used for constant volume; the acetonitrile solution was then transferred to a sample vial after passing through a 0.45 μm organic filter head and measured using a gas chromatograph equipped with mass spectrometry.
Preferably, in step 3), the measurement conditions of the GC-MS are:
preferably, in step 4), the concentration of acetophenone in the extraction solution is converted to the content of acetophenone in the sample, and the amount is quantified by an external standard method according to a solvent calibration curve, with a minimum quantitative concentration of 2mg/kg.
Compared with the prior art, the invention provides a method for measuring the content of the acetophenone in the plastics, the chloroprene rubber and the foam by using an organic solvent extraction and a gas chromatograph-mass spectrometer (hereinafter referred to as GC-MS), the measuring method is quick and simple, the accurate measurement of the content of the acetophenone in the plastics, the chloroprene rubber and the foam can be realized, the minimum quantitative concentration is 2mg/kg, the problem that no method for detecting the content of the acetophenone is solved, the requirement for monitoring and controlling the content of the acetophenone in the plastics, the chloroprene rubber and the foam is completely met, and the method is worthy of popularization and application.
[ Description of the drawings ]
FIG. 1 is a TIC chromatogram obtained by detecting the content of acetophenone in a neoprene sample by a gas chromatograph-mass spectrometer according to example 1 of the present invention;
FIG. 2 is a TIC chromatogram obtained by detecting the content of acetophenone in a foam sample by a gas chromatograph-mass spectrometer according to example 2 of the present invention;
FIG. 3 is a TIC chromatogram of the present invention (13.8 min peak indicates that the compound is acetophenone).
Detailed description of the preferred embodiments
The invention provides a method for directly measuring the content of the acetophenone in plastics, neoprene and foam by GC-MS through extraction aiming at the problem that the content of the acetophenone is detected although the acetophenone is added. The principle of the invention is as follows: the method comprises the steps of ultrasonically extracting the acetophenone azine in plastic, chloroprene rubber and foam samples by using an organic solution, concentrating, fixing the volume, filtering, and then analyzing and testing by using GC-MS.
The method for measuring the content of the acetophenone azine in the plastic, the chloroprene rubber and the foam comprises the following steps: 1) Sample pretreatment: cutting the sample into small pieces by scissors, uniformly mixing the crushed sample, and filling the mixture into a clean and dry self-sealing bag for sealing and preserving for later use; after mixing, 0.50g of sample was weighed accurately into a 50mL centrifuge tube. 2) Extraction of the sample: adding normal hexane into the plastic and chloroprene rubber samples for ultrasonic extraction; transferring the foam sample into a needle tube with a needle removed, and adding n-hexane for ultrasonic extraction; the extract was distilled to near dryness, fixed in volume with acetonitrile, filtered and measured by gas chromatograph equipped with mass spectrum. 3) The concentration of acetophenone in the sample extraction solution obtained in step 2) was measured by a gas chromatography-mass spectrometry (hereinafter referred to as GC-MS) method. 4) Calculating the content of the acetophenone in the sample according to the concentration of the acetophenone in the sample extraction solution obtained in the step 3).
The invention is further described below with reference to specific examples.
Example 1: determination of the content of Acetylbenzazine in Neoprene
(1) Sample pretreatment: cutting textile sample with scissors, or pulverizing foam sample with pulverizer, wherein the size of sample is not more than 2mm×2mm; mixing the crushed materials, and packaging into clean and dry self-sealing bags, and sealing for later use; after mixing, 0.50 g.+ -. 0.01g of sample is weighed accurately into a 50mL centrifuge tube.
(2) Extraction of the sample: 5mL of normal hexane is added into a centrifuge tube filled with a sample, and the mixture is subjected to ultrasonic treatment at room temperature for 30min, and the extract is completely transferred into a 50mL flat-bottomed flask; the centrifuge tube is washed by 5mL of normal hexane, the solution is combined into a flat-bottomed flask, the mixture is steamed to be nearly dry, and 1mL of acetonitrile is used for constant volume; the acetonitrile solution was transferred to a sample injection vial after passing through a 0.45 μm organic filter head, and tested on-press using a gas chromatograph equipped with mass spectrometry.
(3) Measuring the concentration of the acetophenone in the sample extraction solution obtained in the step (2) by adopting a gas chromatography-mass spectrometry (hereinafter referred to as GC-MS) method; the GC-MS measurement conditions were:
(4) The concentration of acetophenone in the extraction solution was converted to the content of acetophenone in the sample, and the method was performed according to a calibration curve using an external standard.
The content of the acetophenone in the butyl cyanide rubber sample was detected to be 8.14mg/kg. As shown in FIG. 1, TIC chromatogram obtained by detecting the content of acetophenone in the neoprene sample by GC-MS is shown. In the figure, 13.8min of the chromatographic peak is the chromatographic peak of the acetophenone in the neoprene extraction solution.
Example 2: determination of the content of Acetobenzazine in foam
(1) Sample pretreatment: cutting textile sample with scissors, or pulverizing foam sample with pulverizer, wherein the size of sample is not more than 2mm×2mm; mixing the crushed materials, and packaging into clean and dry self-sealing bags, and sealing for later use; after mixing, 0.50 g.+ -. 0.01g of sample is weighed accurately into a 50mL centrifuge tube.
(2) Extraction of the sample: adding 15mL of normal hexane into the sample for extraction, completely transferring the extract to a 50mL flat-bottomed flask after ultrasonic treatment at room temperature for 30min, transferring the sample into a needle tube with a needle removed, extruding the sample by using a push rod, and extruding the extract absorbed by the sample into the flat-bottomed flask as much as possible; the centrifuge tube is washed by 5mL of normal hexane, the solution is combined into a flat-bottomed flask, the mixture is steamed to be nearly dry, and 1mL of acetonitrile is used for constant volume; the acetonitrile solution was transferred to a sample vial after passing through a 0.45 μm organic filter head and measured using a gas chromatograph equipped with mass spectrometry.
(3) Measuring the concentration of the acetophenone in the sample extraction solution obtained in the step (2) by adopting a gas chromatography-mass spectrometry (hereinafter referred to as GC-MS) method; the GC-MS measurement conditions were:
(4) The concentration of acetophenone in the extraction solution was converted to the content of acetophenone in the sample, and the method was performed according to a calibration curve using an external standard.
The detection shows that the content of the acetophenone azine in the foam sample is less than 2mg/kg. As shown in FIG. 2, TIC chromatogram obtained by detecting the content of acetophenone in the foam sample by GC-MS was shown. In the figure, the 13.8min chromatographic peak is that of the acetophenone in the foam extraction solution.
The present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the invention are intended to be equivalent substitutes and are included in the scope of the invention.
Claims (3)
1. A method for determining the content of acetophenone azine in plastics, neoprene or foam, comprising the steps of:
1) Sample pretreatment: crushing the sample by a crusher, uniformly mixing the crushed sample, and filling the mixture into a clean and dry self-sealing bag for sealing and preserving for later use; accurately weighing a proper amount of sample in a centrifuge tube after uniformly mixing; the sample is a plastic sample, a chloroprene rubber sample or a foam sample;
2) Extraction of the sample:
Adding 5mL of normal hexane into a plastic sample or a chloroprene rubber sample for extraction, completely transferring the extract to a 50mL flat-bottomed flask after ultrasonic treatment at room temperature for 30min, washing a centrifuge tube with 5mL of normal hexane, merging the solutions into the flat-bottomed flask, performing rotary evaporation until the solution is nearly dry, and fixing the volume with 1mL of acetonitrile; then acetonitrile solution is transferred to a sample injection small bottle after passing through a 0.45 mu m organic filter head, and is measured by a gas chromatograph with mass spectrum;
Adding 15mL of normal hexane into the foam sample for extraction, completely transferring the extract to a 50mL flat-bottomed flask after ultrasonic treatment at room temperature for 30min, transferring the sample into a needle tube with a needle removed, extruding the sample by using a push rod, and extruding the extract absorbed by the sample into the flat-bottomed flask as much as possible; the centrifuge tube is washed by 5mL of normal hexane, the solution is combined into a flat-bottomed flask, the mixture is steamed to be nearly dry, and 1mL of acetonitrile is used for constant volume; then acetonitrile solution is transferred to a sample injection small bottle after passing through a 0.45 mu m organic filter head, and is measured by a gas chromatograph with mass spectrum;
3) Determining the concentration of the acetophenone in the sample extraction solution obtained in the step 2) by adopting a GC-MS gas chromatography-mass spectrometry method;
4) Calculating the content of the acetophenone in the sample according to the concentration of the acetophenone in the sample extraction solution obtained in the step 3);
in step 3), the measurement conditions of the GC-MS are as follows:
instrument: agilent 6890/5975B gas chromatograph-mass spectrometer;
sample injection mode and sample injection amount: sample introduction is not carried out in a split way, and 1.0 mu l of sample introduction is carried out;
analytical column and model: DB-5MS 30m x 0.25mm x 0.25 μm;
sample inlet temperature: 200 ℃;
carrier gas flow rate: 1.0mL/min;
chromatographic column initial temperature and hold time: for 0min at 100deg.C;
chromatographic column temperature program: (1) a temperature value of 100 ℃ and a holding time of 0min; (2) Heating rate of 10deg.C/min, temperature value of 300deg.C, and holding time of 5min;
Detector temperature: 230 ℃;
full SCAN detection SCAN: scanning time is 4.00-25.00 min, and scanning ion m/z is 40-400;
selecting an ion detection SIM: the scanning time is 4.00-25.00 min, and the scanning ion m/z is 77, 221, 236.
2. The method of claim 1, wherein: in step 1), the sample is crushed into small pieces of 2X 2mm by a crusher; after mixing, 0.50 g.+ -. 0.01g of sample is weighed accurately into a 50mL centrifuge tube.
3. The method of claim 1, wherein: in step 4), the concentration of the acetophenone in the extraction solution is converted to the content of the acetophenone in the sample, and the content is quantified by an external standard method according to a solvent calibration curve, wherein the minimum quantification concentration is 2mg/kg.
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