CN108627371B - Method for extracting polycyclic aromatic hydrocarbon from PC/POE product - Google Patents

Abstract

The invention discloses a method for extracting polycyclic aromatic hydrocarbon from a PC/POE product, which comprises the following steps: a. crushing the PC/POE product to obtain a particle sample; b. weighing a predetermined amount of crushed particle samples into a headspace sample bottle, adding an activating agent, capping, and performing ultrasonic forming on suspension in a water bath at 55-65 ℃ to form suspension; c. after the cover is opened, a predetermined amount of turbid liquid is measured and slowly dripped into an extraction container filled with a polar purifying agent and a reverse phase extraction coagulating agent in a tube, and after vortex mixing, supernatant liquid is extracted by centrifugation or negative pressure. The extraction method provided by the invention has the characteristics of rapidness, simplicity, low cost, less interference, small instrument loss and the like.

Description

Method for extracting polycyclic aromatic hydrocarbon from PC/POE product

Technical Field

The invention relates to the extraction of polycyclic aromatic hydrocarbon in plastic products in the fields of machinery, food, environment, automobiles, home furnishing and the like; in particular to a method for extracting polycyclic aromatic hydrocarbon in PC or POE products by a PPME polar mixed reversed phase extraction method.

Background

Polycyclic Aromatic Hydrocarbons (PAHs) refer to a series of hydrocarbon compounds formed by arranging two or more benzene rings together in a linear, angular or cluster shape, are a class of persistent organic pollutants with carcinogenesis, teratogenesis and genogenic mutation commonly existing in the current environment, and are easy to accumulate in organisms due to stable properties, thereby drawing wide attention of people.

Because many plastic products have excellent properties such as acid and alkali resistance, wear resistance, flame resistance and the like, the plastic products are widely applied to toys, plastic particles, daily necessities and leather. PC (polycarbonate) is a high molecular polymer containing carbonate groups in its molecular chain, and is classified into various types such as aliphatic, aromatic, aliphatic-aromatic, and the like, depending on the structure of the ester groups. Among them, aliphatic and aliphatic-aromatic polycarbonates have limited their use as engineering plastics due to their low mechanical properties. Only aromatic polycarbonates are currently produced industrially. Due to the structural particularity of polycarbonate, the polycarbonate is the universal engineering plastic with the highest growth speed in five engineering plastics. PC is a linear carbonate polyester in which the carbonate groups alternate with other groups, either aromatic or aliphatic, or both. Bisphenol a type PC is the most important industrial product. Colorless and transparent, heat-resistant, impact-resistant and flame-retardant BI grade, and has good mechanical properties at common use temperature. Research shows that the PC product is one of important existing carriers of the polycyclic aromatic hydrocarbon, the sample matrix of the PC product is complex, the number of interferents is large, direct extraction is difficult, and analysis can be carried out only after sample pretreatment.

The POE plastic raw material is generally from petrochemicals which take petroleum or natural gas as raw materials and is a high molecular resin obtained through polymerization, ethylene-octene copolymer elastomer (POE) is used as a copolymer of ethylene and octene, the content of octene is usually more than 20%, polyethylene chain segments are crystalline, but due to the intervention of octene, the crystallization of part of polyethylene is damaged, the octene chain segments and amorphous polyethylene chain segments jointly form an elastic amorphous region (rubber phase), and the rest polyethylene crystalline part forms a resin phase and plays a role of a physical crosslinking point. POE not only has excellent toughness, but also improves the rheological property of the polymer during processing, and simultaneously improves the transparency of the material; the POE product is one of important existing carriers of the polycyclic aromatic hydrocarbon, and the POE product has complex sample matrix, more interferents and difficult direct extraction, and can be analyzed only after sample pretreatment.

At present, the extraction method of polycyclic aromatic hydrocarbon in plastic products mainly comprises the steps of extracting by using an organic solvent, carrying out solid-phase extraction and purification, and then measuring by using methods such as gas chromatography, high performance liquid chromatography, gas chromatography-mass spectrometry and the like. The main methods for extracting polycyclic aromatic hydrocarbon include Soxhlet extraction method, ultrasonic extraction method, supercritical fluid extraction method and microwave extraction method. These extraction methods have the following disadvantages in the specific experimental procedures: 1) the Soxhlet extraction method is complex to operate, continuous extraction is generally needed, the extraction time is long, the Soxhlet extraction effect of the polycyclic aromatic hydrocarbon in the plastic product is generally better for 20-30 times, and a large amount of toxic organic solvent is needed. 2) According to the method for measuring polycyclic aromatic hydrocarbon in SN/T1877.2-2007 plastic raw materials and products thereof and other literatures, liquid nitrogen is adopted for freezing and crushing, and n-hexane/acetone or n-hexane/dichloromethane is added as an extraction solution for microwave extraction. The experimental cost of the liquid nitrogen freezing and crushing method used by the method is high, the extracted solution can only swell the plastic product to the maximum extent, but can not damage the internal structure of the plastic, and the extraction efficiency is greatly reduced. The extraction solution is often turbid, and it is difficult to extract the supernatant and to smoothly perform solid-phase extraction. 3) According to the pretreatment scheme in GB/T29784.2-2013, toluene is used as an extraction solution, and experiments prove that the toluene only has a good dissolving effect on PC raw materials and products thereof under specified extraction conditions, but the dissolution solution contains a plurality of high polymers and ester plasticizing aids such as phthalate esters and sebacic esters. The content of the substances in plastic products is generally high, the main interference is generated in the process of qualitatively and quantitatively determining the polycyclic aromatic hydrocarbon, the interference can not be well eliminated by using solid phase extraction purification methods such as silica gel/alumina columns and the like, and the solid phase extraction purification operation is time-consuming and tedious. If the purification process of solid phase extraction is not adopted for direct sample injection detection, the sensitivity and the service life of a chromatographic column and an instrument core component can be greatly reduced. Therefore, it is necessary to establish a technology for extracting polycyclic aromatic hydrocarbons from plastic products with rapidness, simplicity, low cost and small interference.

Conventional pretreatment methods include Solid Phase Extraction (SPE), distributed solid phase extraction (d-SPE), and liquid-liquid extraction (LL E).

Liquid-liquid extraction remains the dominant sample pretreatment method in many laboratories. Liquid-liquid extraction involves two liquid phases that are poorly soluble in each other. Typically one liquid phase is an aqueous solvent and the other liquid phase is an organic solvent that is not or poorly water soluble. The extraction separation of the target compound is achieved by utilizing different partition rates of the target compound in two liquid phases.

Solid phase extraction is a current pretreatment method for purifying liquid samples with solid adsorbents. The main core principle is that solid adsorbent is packed in a needle cylinder column, sample solution is made to pass through adsorbent bed, and the compounds in the sample are adsorbed to solute via adsorbent or retained on the adsorbent. In solid phase extraction, the solid phase adsorbs more of the isolate than the solvent that dissolves the isolate. The adsorption force is mainly divided into nonpolar acting force, polar acting force, ionic acting force, covalent acting force and various acting forces. When the sample solution is passed through the adsorbent bed, the isolate is concentrated on its surface and the other sample components are passed through the adsorbent bed, and a high purity and concentrated isolate can be obtained by the adsorbent adsorbing only the isolate and not the other sample components. The adsorbent filler is used for adsorbing impurities by utilizing the interaction of the adsorbent filler and the impurities in the matrix, so that the purposes of impurity removal and purification are achieved. The dispersive solid phase extraction is to disperse solid phase extraction adsorbent particles in the extraction liquid of a sample, and to adsorb impurities in the extraction liquid by using the dispersed solid phase extraction adsorbent, thereby achieving the purpose of purifying the extraction liquid.

The invention provides a method for extracting polycyclic aromatic hydrocarbon from plastic products, which comprises the steps of (1) crushing and weighing a plastic product sample, wrapping the plastic product sample in filter paper, placing the plastic product sample in a sample bottle, adding a main and auxiliary extracting agent 20m L of acetone and dichloromethane in a volume ratio of 1:1, carrying out ultrasonic extraction for 60-80min, (2) purifying, absorbing polycyclic aromatic hydrocarbon in extraction liquid by floride diatomite in a chromatographic column, eluting, collecting, concentrating eluent, and fixing volume, and (3) measuring a sample by adopting a gas chromatography, and qualitatively and quantitatively analyzing polycyclic aromatic hydrocarbon components.

Therefore, there is a need to provide a method for extracting polycyclic aromatic hydrocarbons from PC/POE products quickly, easily, inexpensively and with less interference.

Disclosure of Invention

The technical problem to be solved by the invention is to provide the method for extracting the polycyclic aromatic hydrocarbon from the PC/POE product, which can be used for extracting the polycyclic aromatic hydrocarbon from the PC or POE product quickly, simply and conveniently with low cost and small interference, and is convenient to popularize and apply.

The technical scheme adopted by the invention for solving the technical problems is to provide a method for extracting polycyclic aromatic hydrocarbon from a PC/POE product, which comprises the following steps: a. crushing a PC or POE product to obtain a particle sample; b. weighing a predetermined amount of crushed particle samples into a headspace sample bottle, adding an activating agent, capping, and performing ultrasonic forming on suspension in a water bath at 55-65 ℃ to form suspension; c. after the cover is opened, a predetermined amount of turbid liquid is measured and slowly dripped into an extraction container filled with a polar purifying agent and a reverse phase extraction coagulating agent in a tube, and after vortex mixing, supernatant liquid is extracted by centrifugation or negative pressure.

Further, in step a, the PC or POE product is pulverized to a particle size of about 0.5cm by a homogenizing mill.

Further, the step b is that 0.50g to 20m L of crushed sample is weighed into a headspace jaw bottle, 10m L of activating agent is added, and ultrasonic treatment is carried out for 40min under water bath at 60 ℃ after capping.

Further, the activator component and the volume ratio in the step b are benzene: 80:20 parts of trichloromethane.

And further, in the step c), the extraction container is an extraction tube, after the extraction tube is covered, 1ml of suspension is measured and slowly dropped into the extraction tube filled with 5m L acetonitrile and 30mg of SPE filler containing a cyano bonding phase, vortex mixing is carried out for 30s, and after centrifugation is carried out for 5min at 4000r/min, a supernatant is obtained.

Furthermore, the extraction container is a special extraction tube, the special extraction tube comprises a tube body, a needle tube-shaped through hole is formed in the bottom of the tube body, the needle tube-shaped through hole is connected with the luer plug or the negative pressure container, and a sieve plate is arranged at the bottom of the tube body.

Further, an upper cover is arranged at the port of the pipe body, a sealing spacer is arranged in the upper cover, and the upper cover and the pipe body are tightly screwed in a sealing mode.

Further, the pipe body is formed by high borosilicate glass at a high temperature in one step.

Furthermore, the sealing spacer is silica gel/PTFE, the luer plug is made of polypropylene, and the sieve plate is made of polyethylene; and an air suction pump is connected above the negative pressure container.

Compared with the prior art, the invention has the following beneficial effects: the extraction method of polycyclic aromatic hydrocarbon in PC or POE products provided by the invention has the following advantages that (1) three pretreatment schemes in the prior art have similar action mechanisms, and the purposes of separation, purification, trace enrichment, desalting and derivation are achieved by utilizing two phases with different properties and in contact with a target compound through selective competition of various physical and chemical acting forces of the target compound.

LL E utilizes the different distribution rate of the target compound in two liquid phases to achieve the extraction separation of the target compound, and for a compound existing in only one chemical form under given conditions, the distribution rate in two immiscible liquid phase systems depends on the selective competition for the thermodynamic properties of the target compound.

The invention innovatively provides a new technical scheme, wherein in a multiphase system, due to the instantaneous difference of thermodynamic acting forces generated by two immiscible organic phases, a flocculated substance of a macromolecular polymer is separated, a target compound is extracted into a polar solution environment, cyano SPE filler in the multiphase system and the compound generate pi-pi bond interaction, dipole-dipole interaction and dipole-induced dipole interaction generate adsorption on a large amount of medium-polarity impurities in POE or PC products, meanwhile, a solid-phase particle, the flocculated substance and a polar solvent are timely acted as a condensation nucleus in a mixed reaction, and after oscillation operation, the solid-phase particle and the flocculated substance quickly form spherical precipitation. Therefore, the purposes of efficiently and quickly removing macromolecular polymers, selectively adsorbing Polar impurities, enriching, purifying and extracting non-Polar or very weak-Polar small molecular target compound supernatant are achieved, the distribution coefficient among phases is determined again, the high extraction efficiency level which cannot be achieved by liquid-liquid extraction is achieved, and the technical scheme is named as Polar mixed reversed phase extraction (Polar mixed phase extraction) PPME (short for PPME) in English due to the interaction among multiphase multi-property systems in the reaction.

(2) The invention adopts benzene: 80 parts of trichloromethane: the activator of 20 is that benzene has strong ability to overcome the aggregation force between POE macromolecules, the benzene can completely dissolve polyolefin elastomer under specific extraction conditions, and POE plastic has excellent toughening effect on PP and better compatibility with PP and active calcium carbonate. The POE plastic has narrow molecular weight distribution, lateral octyl groups in the molecular structure are longer than lateral ethyl groups, and a connecting point can be formed in the molecular structure, so that the components play a role in connecting and buffering, the system plays a role in dispersing and buffering impact energy when impacted, the probability of crack development caused by stress is reduced, and the impact strength of the system is improved. When the system is under tension, the network structure formed by the bond points can be greatly deformed, so that the elongation at break of the system is remarkably increased, and when the content of the POE plastic is increased, the tensile strength, the bending strength and the bending modulus of the system are all reduced, which are determined by the properties of the POE plastic, so that the content of the POE plastic is controlled to be below 20 percent. The trichloromethane has excellent solubility for the crosslinking matrix components such as lipids and olefins in the POE product.

Polycarbonate (abbreviated as PC) is a high molecular polymer containing carbonate groups in molecular chains, is a tough thermoplastic resin, is named from CO3 groups in the polycarbonate, is synthesized by bisphenol A and diphenyl carbonate through ester exchange and polycondensation reaction, however, the high molecular chains forming the PC have large difference in polarity, and are difficult to dissolve by a single solvent. For this purpose, multi-component mixed solvents are used to achieve complete dissolution of PC.

It is known from the molecular structure and synthesis process of the polymer constituting PC that polycarbonate (PC for short) is synthesized from bisphenol a and diphenyl carbonate by transesterification and polycondensation, and is classified into aliphatic and aromatic types according to the alcohol structure, PC is a linear carbonate polyester in which the carbonate groups alternate with other groups, which may be aromatic, aliphatic or both. Benzene is used as a common breaking agent and is a strong solvent of ester substances, and trichloromethane has strong polarity and active chemical property due to the induction effect of three chlorine atoms and can dissolve high polymer materials such as plastics, organic glass, rubber and the like, so that benzene is selected: and (3) taking a mixed solvent of 80:20 trichloromethane as a main solvent.

(3) The key technology of the invention is to creatively develop a method for rapidly precipitating the high molecular polymer in the immiscible solvent, because the POE or PC high molecular polymer is prepared in the following steps: in the reaction of the chloroform-80: 20 activating agent and the acetonitrile polar purifying agent, the flocculated substances of the macromolecular polymer are separated out due to the instantaneous difference of thermodynamic forces generated by two immiscible organic phases. And the purifying agent is a polar solution, so that a good reaction system is provided for subsequent reversed-phase extraction.

(4) The solid phase extraction method of polycyclic aromatic hydrocarbon in POE and POE products is a reverse phase extraction process of normal phase cyano-group filling material. Because of the presence of polar functional groups, this silica gel is more adsorptive than reverse phase silica gel. The normal phase filler containing the cyano is very suitable for reverse phase extraction of compounds with some medium polarity impurities, and can adsorb a large amount of medium polarity impurities in POE or PC products.

(5) A large amount of medium polar compounds existing in PC or POE products can be adsorbed by cyano-group fillers, such as additive flame retardant Sb in PC or POE products₂O₃And the surface of the PC or POE material is damaged. Meanwhile, the solid-phase particles can act as coagulation nuclei in the reaction with the flocculent substance and the polar solution timely, and the coagulation nuclei can be quickly reacted with the flocculent substance and the polar solution after oscillation operationThe flocculated material forms a spherical precipitate. Therefore, the purposes of removing macromolecular polymers, selectively adsorbing impurities, enriching, purifying and extracting small molecular target supernatant can be efficiently and quickly achieved, the distribution coefficient among all phases can be determined again, and the high extraction efficiency level which cannot be achieved by liquid-liquid extraction can be achieved.

(6) The current special polycyclic aromatic hydrocarbon SPE column is a reversed phase SPE column, the action mechanism is that when template molecules (imprinted molecules) contact with polymer monomers, multiple action points are formed, the action can be memorized through the polymerization process, and after the template molecules are removed, cavities which are matched with the space configuration of the template molecules and have the multiple action points are formed in the polymers, and the cavities have the selective recognition characteristic on the template molecules and analogues thereof. The extraction method utilizes the combined action mechanism of molecular imprinting and reverse phase extraction to adsorb polycyclic aromatic hydrocarbon, and the normal phase SPE particles selected by the extraction method only can adsorb some medium polarity impurities existing in PC or POE products and have no adsorption effect on nonpolar or weak polarity PAHs

(7) The extraction method provided by the invention fully embodies the characteristics of rapidness, simplicity, convenience, low cost, less interference, small instrument loss and the like. Wherein 'fast' is reflected in that the operation time of the whole experiment is 1.5 h; the 'simplicity' is embodied in that the pretreatment method only involves the extraction of a plurality of reagents and the mixing and centrifugation of an extraction tube; the low cost is embodied in that only common instruments such as an ultrasonic oscillator, a centrifuge, a gas analyzer and the like are needed in the experiment; the less interference is reflected in less impurities in chromatogram analysis, and is beneficial to qualitative and quantitative analysis of polycyclic aromatic hydrocarbon; the 'small loss to the instrument' is reflected in that the sample injection solution is shown as clear supernatant after NPME treatment, and the loss to the instrument parts is very little.

Drawings

FIG. 1 is a schematic view of the overall structure of the PAHs extraction tube of the present invention;

FIG. 2 is an exploded view of the PAHs extraction tube of the present invention;

FIG. 3 is a GC-MS chromatogram of a 100. mu.g/L polycyclic aromatic hydrocarbon according to the invention;

FIG. 4 is a GC-MS chromatogram of a POE automobile accessory article matrix blank in an embodiment of the invention;

FIG. 5 is a GC-MS chromatogram of POE automobile accessory product labeled with 1 μ g/m L in the example of the invention;

FIG. 6 is a blank GC-MS chromatogram of a substrate from a PC machine housing article according to another embodiment of the present invention;

FIG. 7 is a GC-MS chromatogram of a PC machine housing spiked with 1 μ g/m L in accordance with another embodiment of the present invention.

In the figure:

1. upper cover 2, sealing spacer 3 and pipe body

4. Sieve plate 5, needle tube-shaped through hole 6 and luer plug

Detailed Description

The invention is further described below with reference to the figures and examples.

The invention provides a method for extracting polycyclic aromatic hydrocarbon from a PC/POE product, which comprises the following steps of: extracting a PC or POE product by using an activating agent of 80:20, then performing polar mixing and reverse-phase extraction by using an innovative PPME, slowly dripping an extract into a purifying agent with acetonitrile as a component, separating out flocculated substances of a macromolecular polymer by using the instantaneous difference of thermodynamic acting forces generated by two immiscible organic phases in a multiphase system, purifying and enriching a target compound by using a reverse-phase extraction process of a normal-phase SPE filler in a polar solvent, and finally taking supernatant after mixing and centrifuging to enter a method for analyzing the content of polycyclic aromatic hydrocarbon by chromatography. .

The technical solution of the present invention is further illustrated by the following specific examples. These examples are merely exemplary applications and are not to be construed as limiting the scope of the invention as claimed.

Example 1

The following example is to extract polycyclic aromatic hydrocarbon from POE automobile accessory products:

POE automobile parts were ground to a particle size of about 0.5cm by 0.5cm using a homogenizer.

The pulverized sample was weighed accurately into a 0.50g to 20m L headspace screw sample bottle, 10m L activator (benzene: chloroform: 80:20) was added, and after capping, sonication was carried out in a water bath at 60 ℃ for 40 min.

After the cover is opened, 1m L suspension is weighed and slowly dropped into an extraction tube filled with 5m L of polar purificant (acetonitrile) and 30mg of reverse phase extraction coagulator (SPE normal phase filler containing cyano), vortex mixing is carried out for 30s, and after centrifugation is carried out for 5min at 4000r/min, supernatant is taken for sample analysis of gas chromatography mass spectrometry.

Referring to fig. 1 and 2, the special extraction tube adopted in the embodiment comprises a tube body 3, an upper cover 1 is arranged at a port of the tube body 3, the upper cover 1 is preferably an aluminum cover, the upper cover 1 and the tube body 3 can be sealed through a jaw, the jaw of the aluminum cover can provide the tightest sealing, the possibility of volatilization of a sample and a reagent is reduced, a sealing spacer 2 is arranged in the upper cover 1, the spacer is made of silica gel/PTFE, the silica gel/PTFE has dense display molecular chains and limits the thermal activity of polymer molecules, so that the air permeability is low, the air tightness is good, the special extraction tube has excellent corrosion resistance, high temperature resistance, non-toxicity and adhesion resistance, good elasticity and sealing performance, is not easy to react with a chemical reagent, the tube body is stable in property, the tube body 3 utilizes the conductive characteristic of high borosilicate glass in a high-temperature state, glass melting is realized by heating in the glass, the borosilicate glass has a very low thermal expansion coefficient which is about one third of common glass, the borosilicate glass, the influence caused by temperature gradient stress is reduced, so that the tube body has stronger anti-fracture performance, 1.0.0.05 mm, the tube wall thickness is uniform, high-speed, the special extraction tube can be used, the bottom of a needle tube is matched with a needle tube, a needle tube is formed by a needle tube, a needle tube is connected with a needle tube, a needle tube is connected with a needle tube, a needle tube with a needle tube.

Example 2

The following example is the extraction of polycyclic aromatic hydrocarbons from PC machine housing products:

the PC tool housing was milled to a particle size of about 0.5cm by 0.5cm using a homogenizer.

The pulverized sample was weighed accurately into a 0.50g to 20m L headspace screw sample bottle, 10m L activator (benzene: chloroform: 80:20) was added, and after capping, sonication was carried out in a water bath at 60 ℃ for 40 min.

After the cover is opened, 1m L suspension is weighed and slowly dropped into an extraction tube filled with 5m L of polar purificant (acetonitrile) and 30mg of reverse phase extraction coagulator (SPE normal phase filler containing cyano), vortex mixing is carried out for 30s, and after centrifugation is carried out for 5min at 4000r/min, supernatant is taken for sample analysis of gas chromatography mass spectrometry.

The detection method comprises the following steps:

set on a gas chromatography mass spectrometer:

chromatographic column CNW CD-5MS, 30m × 0.25mm × 0.25.25 μm

Carrier gas He, column flow 2.0m L/min

And (3) sample introduction mode: non-shunting pulse sample introduction

Pulse voltage: 45.00kpa

Sample inlet temperature: 280 deg.C

Transmission line temperature: 300 deg.C

Ion source temperature: 280 deg.C

Ionization energy: 70Ev

Solvent retardation: 4.5min

Ion monitoring mode: selective ion Scanning (SIM)

Target object	Quantitative ion
		Naphthalene	128
Acenaphthylene	152
		Acenaphthene	152
Fluorene compounds	166
		Phenanthrene	178
Anthracene	178
		Fluoranthene	202
Pyrene	202
		1, 2-benzo [ A ]]Anthracene	228
Flexion type	228
		Benzo (B) fluoranthene	252
Benzo [ k ] benzene]Fluoranthene	252
		Benzo (a) pyrene	252
Indeno (1,2,3-CD) ratio	276
		Diphenyl anthracenes	276
Benzo (G, H, I) perylenes	276

Temperature programming: the initial temperature is 50 ℃, the temperature is kept for 1min, the temperature is raised to 200 ℃ at the speed of 25 ℃/min, the temperature is raised to 250 ℃ at the speed of 10 ℃/min, and the temperature is raised to 300 ℃ at the speed of 5 ℃/min and kept for 5 min.

FIG. 3 is a GC-MS chromatogram of 100. mu.g/L polycyclic aromatic hydrocarbon, which shows that 100. mu.g/L polycyclic aromatic hydrocarbon standard has good peak appearance on GC-MS.

FIG. 4 is a blank GC-MS chromatogram of the POE product matrix in example 1 of the present invention; the POE product can remove most impurities under the treatment of the method, and the residual impurities do not interfere the qualitative and quantitative determination of the subsequent target.

FIG. 5 is a GC-MS chromatogram of POE product labeled with 1 μ g/m L in example 1 of the present invention, which shows that the POE product labeled with the peak is good and the recovery rate of the method can be examined with the chromatogram of the polycyclic aromatic hydrocarbon standard.

FIG. 6 is a blank GC-MS chromatogram of a substrate from a PC machine housing article according to example 2 of the present invention; the PC machine shell product can remove most impurities under the treatment of the method, and the residual impurities do not interfere with the qualitative and quantitative determination of the subsequent target.

FIG. 7 is a GC-MS chromatogram of 1 μ g/m L GC-MS of the PC machine shell label in example 2 of the present invention, which shows that the PC machine shell product has good peak labeling and can be examined for recovery rate with the chromatogram of the polycyclic aromatic hydrocarbon standard.

The abscissa of the above graph represents the peak time (min) and the ordinate represents the response value of the compound.

Therefore, the extraction method of the invention can obtain the required measuring result completely by a common biochemical analyzer, has high sensitivity and accuracy, is not polluted by internal and external substances, and is convenient for popularization and application.

Although the present invention has been described with respect to the preferred embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (7)

1. A method for extracting polycyclic aromatic hydrocarbon from a PC/POE product is characterized by comprising the following steps:

a. crushing a PC or POE product to obtain a particle sample;

b. weighing a predetermined amount of crushed particle samples into a headspace sample bottle, adding an activating agent, capping, and performing ultrasonic forming on suspension in a water bath at 55-65 ℃ to form suspension;

c. after the cover is opened, a predetermined amount of turbid liquid is measured and slowly dripped into an extraction container filled with a polar purifying agent and a reverse-phase extraction coagulating agent in a tube, and after vortex mixing, supernatant liquid is extracted by centrifugation or negative pressure;

the activating agent component and the volume ratio in the step b are benzene: chloroform =80: 20;

and c, taking the extraction container as an extraction tube, measuring 1m of suspension of L after the extraction container is opened, slowly dripping the suspension into the extraction tube filled with 5m of L acetonitrile and 30mg of SPE filler containing a cyano bonding phase, mixing the mixture by vortex for 30s, centrifuging the mixture for 5min at 4000r/min, and taking supernatant.

2. The extraction process of claim 1, wherein the PC or POE product is milled to a particle size of about 0.5cm by 0.5cm in step a using a homogenizer.

3. The extraction method of claim 1, wherein the step b comprises weighing the pulverized sample 0.50g to 20m L headspace bottles, adding 10m L activator, capping, and performing ultrasonic treatment in 60 deg.C water bath for 40 min.

4. The extraction method as claimed in claim 1, wherein the extraction container is a dedicated extraction tube, the dedicated extraction tube comprises a tube body, a needle tube-shaped through hole is formed at the bottom of the tube body, the needle tube-shaped through hole is connected with a luer plug or a negative pressure container, and a sieve plate is arranged at the bottom of the tube body.

5. The extraction method according to claim 4, wherein the end of the tube body is provided with an upper cover, a sealing spacer is arranged in the upper cover, and the upper cover is tightly screwed with the tube body in a sealing manner.

6. The extraction process of claim 4 wherein the tube is formed in one piece from high temperature borosilicate glass.

7. The extraction process of claim 5, wherein the sealing spacer is silica gel/PTFE, the luer plug is made of polypropylene, and the sieve plate is made of polyethylene; and an air suction pump is connected above the negative pressure container.

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