CN114563508A - Method for purifying polycyclic aromatic hydrocarbon in meat-containing sample and method for detecting polycyclic aromatic hydrocarbon in meat-containing sample - Google Patents
Method for purifying polycyclic aromatic hydrocarbon in meat-containing sample and method for detecting polycyclic aromatic hydrocarbon in meat-containing sample Download PDFInfo
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- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 94
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- 238000001514 detection method Methods 0.000 claims abstract description 27
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- 230000010355 oscillation Effects 0.000 claims description 6
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Images
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
- 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
- G01N30/74—Optical detectors
-
- 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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
Abstract
The invention relates to the technical field of detection of harmful substances in food, in particular to a method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample and a method for detecting polycyclic aromatic hydrocarbon in the meat-containing sample. The purification method provided by the invention comprises the following steps: mixing and grinding a meat-containing sample and chromatographically pure diatomite to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products; mixing and extracting the ground material and an organic extraction solvent, wherein an extracted organic phase is a crude polycyclic aromatic hydrocarbon product, and the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane; and purifying the crude polycyclic aromatic hydrocarbon by using a polycyclic aromatic hydrocarbon molecularly imprinted column, wherein the purified eluent comprises dichloromethane. The purification method provided by the invention can effectively separate the impurities in the meat-containing sample from the polycyclic aromatic hydrocarbon. The preparation method provided by the invention is simple and easy to operate.
Description
Technical Field
The invention relates to the technical field of detection of harmful substances in food, in particular to a method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample and a method for detecting polycyclic aromatic hydrocarbon in the meat-containing sample.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) refer to aromatic hydrocarbons containing two or more benzene rings. They mainly have two combination modes, one is non-fused ring type, which comprises biphenyl, biphenylene and polyphenyl fat; the other is fused ring type, which contains hydrocarbons with two carbon atoms shared by two benzene rings, and specifically comprises more than 150 kinds of compounds such as herba Anthragmae, herba phenanthrene, and pyrene. PAHs are considered to be a main organic pollutant affecting human health because of toxicity, genetic toxicity, mutagenicity and carcinogenicity, and can cause various damages to human bodies, such as damages to respiratory systems, circulatory systems and nervous systems and damages to livers and kidneys.
For non-professional workers and non-smokers, more than 70% of polycyclic aromatic hydrocarbon exposure is derived from diet, especially meat products. The content of PAHs in various meat products is significantly higher than other non-meat food products in food of the same quality. Therefore, in view of the importance of the meat products in daily life, the detection of the content of PAHs in the meat products is of great significance to the safety guarantee of the meat products.
The existing methods for analyzing and measuring the polycyclic aromatic hydrocarbon comprise methods such as paper chromatography, thin layer chromatography, packed column gas chromatography, capillary column gas chromatography, gas chromatography-mass spectrometry, high performance liquid chromatography-fluorescence detection method and the like. The methods such as paper chromatography, thin layer chromatography, packed column gas chromatography, etc. can perform quantitative analysis, but the separation efficiency and analysis speed are poor. The gas chromatography-mass spectrometry (GC/MS) and the high performance liquid chromatography-fluorescence detection (HPLC-FLD) have the advantages of high resolution, high sensitivity, wide linear range and good quantitative accuracy, and are the most common terminal detection technologies.
Aiming at the measurement of the content of PAHs in meat products, the meat products need to be pretreated before the measurement of the content of PAHs, impurities in the meat products are removed, and accurate detection results are obtained from the obtained purified PAHs samples to be detected.
The extraction and purification method of PAHs comprises the following steps: soxhlet extraction, ultrasonic extraction, microwave extraction, accelerated solvent extraction, supercritical fluid extraction and synergistic extraction techniques. Due to the high complexity of meat and meat product substrates, cumbersome extraction and purification procedures are usually required to destroy the lipid components and facilitate the extraction of target analytes, so that their pretreatment is more difficult than the pretreatment of other non-fat food samples, and the development of a simple, rapid and efficient pretreatment method is the development direction of analysis techniques for polycyclic aromatic hydrocarbons in meat products.
Molecular imprinting polymerization (MISPE) columns are used for removing impurities due to their selectivity, and have been developed in recent years for use in PAHs pretreatment of meat products in combination with Ultrasonic Extraction (UE). The patent refers to the field of ' determination of polycyclic aromatic hydrocarbon content in meat by gas chromatography-isotope dilution mass spectrometry ' (Yingshan, Liyongli, Chenying, Lijie, food science, 2019,10(12): 321-325) ') and discloses the GC/MS detection of purified products obtained by ultrasonic extraction with n-hexane-dichloromethane and purification with a molecular imprinting column. However, when the detection method in the above article is repeated, it is found that the purification treatment method still exists in the prior art, and particularly, when the detection is carried out on the meat product treated by the purification treatment method, the column efficiency is easily reduced due to the matrix effect, and the detection sensitivity is rapidly reduced.
Disclosure of Invention
In view of the above, the invention provides a method for purifying polycyclic aromatic hydrocarbons in a meat-containing sample and a method for detecting polycyclic aromatic hydrocarbons in a meat-containing sample, the PAHs sample obtained by the purification method provided by the invention has low impurity content and simple method, and when GC/MS detection or HPLC-FLD detection is carried out, the matrix effect is small, and the detection quantitative limit is low.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample, which comprises the following steps:
mixing and grinding a meat-containing sample and chromatographically pure diatomite to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products;
mixing and extracting the ground material and an organic extraction solvent, wherein an extracted organic phase is a crude polycyclic aromatic hydrocarbon product, and the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane;
and purifying the crude polycyclic aromatic hydrocarbon by using a polycyclic aromatic hydrocarbon molecularly imprinted column, wherein the purified eluent comprises dichloromethane.
Preferably, the mass ratio of the meat-containing sample to the chromatographic pure diatomite is less than or equal to 1: 1.
Preferably, the raw material of the mixed grinding also comprises a solid desiccant, and the mass ratio of the solid desiccant to the diatomite is preferably 1: 1.
Preferably, the volume ratio of the dichloromethane to the n-hexane in the mixed solvent of the dichloromethane and the n-hexane is more than or equal to 0.5: 1.
Preferably, the mixing extraction is performed for 2-3 times, and the volume ratio of the mass of the ground material to the volume of the organic extraction solvent is 5g:20mL during each mixing extraction.
Preferably, the mixed extraction is performed under the condition of vortex oscillation, and the time of the vortex oscillation is 30s in each mixed extraction.
Preferably, after each mixing extraction, an extraction suspension is obtained, after the mixing extraction, the method further comprises the steps of sequentially carrying out solid-liquid separation on the extraction suspensions to obtain extraction organic phases, combining the extraction organic phases, and then concentrating to obtain the crude polycyclic aromatic hydrocarbon product, wherein the solid-liquid separation is centrifugation, the rotation speed of the centrifugation is 4500r/min, the centrifugation time is 10min, and during the centrifugation, the temperature of the extraction suspension is-20-normal temperature.
Preferably, the concentration is rotary evaporation drying, and the concentration temperature is 36-40 ℃.
The invention provides a method for detecting polycyclic aromatic hydrocarbons in a meat-containing sample, which is characterized in that a gas chromatography-mass spectrometry method or a high performance liquid chromatography-fluorescence detection method is adopted to detect the purified meat-containing sample, and the purified meat-containing sample is obtained by the purification method of the technical scheme.
Preferably, the polycyclic aromatic hydrocarbon includes naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a]Anthracene,
Benzo [ b ]]Fluoranthene, benzo [ k ]]Fluoranthene, benzo [ a ]]Pyrene, indene benzene [1,2,3-cd]Pyrene, dibenzo [ a, h ]]Anthracene and benzo [ g, h, i ]]One or more of perylene.
The invention provides a method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample, which comprises the following steps: mixing and grinding a meat-containing sample and chromatographically pure diatomite to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products; mixing and extracting the ground material and an organic extraction solvent, wherein an extracted organic phase is a crude polycyclic aromatic hydrocarbon product, and the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane; and purifying the crude polycyclic aromatic hydrocarbon by using a polycyclic aromatic hydrocarbon molecular imprinting column, wherein the purified eluent comprises dichloromethane. The purification method provided by the invention comprises the steps of firstly, adsorbing polycyclic aromatic hydrocarbon in a meat sample by using diatomite in a grinding process, and primarily separating the polycyclic aromatic hydrocarbon from impurities in the meat sample; and then mixing the ground material with an organic solvent, and extracting the ground material by adopting a solid-phase matrix dispersion suspension liquid extraction mode, wherein when the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane, the polycyclic aromatic hydrocarbon can fully enter the organic extraction solvent, the separation rate of the polycyclic aromatic hydrocarbon from impurities in a meat-containing sample is high, and the extraction recovery rate is high, and after a polycyclic aromatic hydrocarbon crude product is obtained, the polycyclic aromatic hydrocarbon molecular imprinting column is adopted to be matched with dichloromethane to be used as an eluent for purification, so that the impurities in the polycyclic aromatic hydrocarbon crude product can be further removed. The purification method provided by the invention can effectively separate the impurities in the meat-containing sample from the polycyclic aromatic hydrocarbon. The preparation method provided by the invention is simple and easy to operate.
The invention provides a method for detecting polycyclic aromatic hydrocarbons in a meat-containing sample, which is characterized in that a gas chromatography-mass spectrometry method or a high performance liquid chromatography-fluorescence detection method is adopted to detect the purified meat-containing sample, and the purified meat-containing sample is obtained by the purification method of the technical scheme. According to the invention, the meat-containing sample extracted and purified by the purification method of the technical scheme is detected, the content of impurities in the sample to be detected is small, the matrix effect is small, the interference of impurities is not easy to occur when GC/MS detection or HPLC-FLD detection is carried out, the reliability is strong, the quantitative limit of detection is low, and the content of 18 polycyclic aromatic hydrocarbons in the meat product can be detected simultaneously.
Drawings
FIG. 1 is a graph of the content of polycyclic aromatic hydrocarbons (labeled 1. mu.g/kg) in a meat sample measured by GC/MS according to an embodiment of the present invention;
wherein 1 is naphthalene, 2 is 1-methylnaphthalene, 3 is 2-methylnaphthalene, 4 is acenaphthylene, 5 is acenaphthylene, 6 is fluorene, 7 is phenanthrene, 8 is anthracene, 9 is fluoranthene, 10 is pyrene, 11 is benzo [ a]Anthracene, 12 is
13 is benzo [ b ]]Fluoranthene, 14 is benzo [ k ]]Fluoranthene, 15 is benzo [ a ]]Pyrene, 16 is indene benzene [1,2,3-cd]Pyrene, 17 is dibenzo [ a, h ]]Anthracene, 18 being benzo [ g, h, i ]]A perylene;
FIG. 2 is a comparison graph of residual interfering substances in the detection of polycyclic aromatic hydrocarbons in cured meat according to the method described in the example of the present invention and the literature "gas chromatography-isotope dilution mass spectrometry" for determining polycyclic aromatic hydrocarbon content in meat "(Yingshan, Liyongli, Chengying, Lijie. food science, 2019,10(12): 321-325).
Detailed Description
The invention provides a method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample, which comprises the following steps:
mixing and grinding a meat-containing sample and chromatographically pure diatomite to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products;
mixing and extracting the ground material and an organic extraction solvent, wherein an extracted organic phase is a crude polycyclic aromatic hydrocarbon product, and the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane;
and purifying the crude polycyclic aromatic hydrocarbon by using a polycyclic aromatic hydrocarbon molecularly imprinted column, wherein the purified eluent comprises dichloromethane.
In the present invention, the starting materials are all commercially available products well known to those skilled in the art, unless otherwise specified.
According to the invention, a meat-containing sample and chromatographic pure diatomite are mixed and ground to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products.
In the present invention, the meat-containing sample comprises meat and/or meat products, preferably meat or meat products.
The present invention preferably pre-treats the meat-containing sample. In the present invention, the pretreatment is preferably a mincing step, and in the present invention, when the meat-containing sample is a frozen sample, the meat-containing sample is preferably thawed before the mincing step. The invention has no special requirements on the concrete implementation process of the mincing, and the meat-containing sample is minced into minced meat.
In a particular embodiment of the invention, the diatomaceous earth is preferably chromatographically pure Florisil diatomaceous earth (LC-Florisil diatomaceous earth).
In the present invention, the mass ratio of the meat-containing sample to diatomaceous earth is preferably 1:1 or less, more preferably 1: 1.
In the present invention, the raw material for mixed grinding preferably further includes a solid desiccant.
In the present invention, the solid desiccant is preferably an analytically pure reagent or a chromatographically pure reagent.
In a particular embodiment of the invention, the solid drying agent is particularly preferably anhydrous sodium sulphate.
In the present invention, the mass ratio of the solid desiccant to the diatomaceous earth is preferably 1: 1.
In a specific embodiment of the invention, the mixed grinding is preferably manual grinding in a mortar.
In the present invention, the time for the mixing and grinding is preferably 10 min.
In the present invention, the temperature of the mixing and polishing is preferably 0 to room temperature.
After the ground material is obtained, the ground material and an organic extraction solvent are mixed and extracted to obtain a crude polycyclic aromatic hydrocarbon product, wherein the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane.
In the present invention, the organic extraction solvent includes dichloromethane or a mixed solvent of dichloromethane and n-hexane, preferably a mixed solvent of dichloromethane and n-hexane.
In the present invention, the volume ratio of dichloromethane to n-hexane in the mixed solvent of dichloromethane and n-hexane is preferably not less than 0.5:1, and more preferably 1: 1.
In the present invention, the number of times of the mixed extraction is preferably 2 to 3 times, and more preferably 2 times.
In the present invention, the ratio of the mass of the ground matter to the volume of the organic extraction solvent is preferably 5g:20mL per mixed extraction.
In the present invention, the mixed extraction is preferably performed under the condition of vortex oscillation, and the time of the vortex oscillation is preferably 30s for each mixed extraction.
In the invention, the extraction suspension is obtained after the mixed extraction, and the invention preferably further comprises the steps of sequentially carrying out solid-liquid separation on the extraction suspension to obtain extraction organic phases, combining the extraction organic phases and concentrating to obtain the crude polycyclic aromatic hydrocarbon.
In the invention, the solid-liquid separation is preferably performed by centrifugation, the rotation speed of the centrifugation is preferably 4500r/min, the time of the centrifugation is preferably 10min, and the temperature of the extraction suspension during the centrifugation is preferably-20 to normal temperature, more preferably-20 to 4 ℃, and most preferably-4 ℃.
In the invention, the solid-liquid separation is carried out to obtain an extraction organic phase and extraction slag.
The extraction slag is used for the next extraction or waste.
The invention combines the extracted organic phases obtained by each solid-liquid separation and then concentrates the organic phases.
In the invention, the concentration is preferably rotary evaporation drying, and the temperature of the concentration is preferably 36-40 ℃, and more preferably 38 ℃.
After the crude polycyclic aromatic hydrocarbon is obtained, the crude polycyclic aromatic hydrocarbon is purified by a polycyclic aromatic hydrocarbon molecularly imprinted column, and the purified eluent comprises dichloromethane.
In the invention, the polycyclic aromatic hydrocarbon molecularly imprinted column is a CNW Poly-Sery polycyclic aromatic hydrocarbon molecularly imprinted column, and the specification is preferably 500mg/6 mL.
In the invention, the polycyclic aromatic hydrocarbon molecularly imprinted column is preferably subjected to pretreatment, and the pretreatment preferably comprises the following steps: and sequentially carrying out activation treatment and balance treatment on the polycyclic aromatic hydrocarbon molecularly imprinted column. In the present invention, the activating solvent for the activating treatment is preferably n-hexane, and the present invention has no particular requirement for the specific implementation process of the mixing treatment, and in the present invention, the solvent for the equilibration treatment is preferably dichloromethane, and the present invention has no particular requirement for the specific implementation process of the equilibration treatment.
Before the polycyclic aromatic hydrocarbon is fed into the column, the polycyclic aromatic hydrocarbon crude product and the organic solvent are preferably mixed to obtain a polycyclic aromatic hydrocarbon crude product solution. The organic solvent in the crude polycyclic aromatic hydrocarbon solution is preferably n-hexane. In the invention, the eluent is preferably dichloromethane, and the volume ratio of the eluent to the crude polycyclic aromatic hydrocarbon solution is preferably 1: 2.
The invention provides a method for detecting polycyclic aromatic hydrocarbons in a meat-containing sample, which is characterized in that a gas chromatography-mass spectrometry method or a high performance liquid chromatography-fluorescence detection method is adopted to detect the purified meat-containing sample, and the purified meat-containing sample is obtained by the purification method of the technical scheme.
In the present invention, when the detection is preferably quantitative detection, the present invention is preferably performed by an internal standard method.
When the internal standard method is adopted for detection, the invention preferably concentrates the purified meat-containing sample obtained by the purification method in the technical scheme in a protective atmosphere, adds an internal standard substance and performs volume fixing to obtain the sample to be detected.
In the present invention, the protective atmosphere is preferably nitrogen.
The invention has no special requirements for the specific implementation process of the concentration.
In the present invention, the volume of the sample to be detected is preferably 0.5 mL.
The invention has no special requirements on the specific implementation process of the gas chromatography-mass spectrometry method or the high performance liquid chromatography-fluorescence detection method.
In the embodiment of the present invention, when the gas chromatography-mass spectrometry is adopted, the present invention preferably adopts a gas chromatography-mass spectrometry combination instrument to detect the sample to be detected.
In the present invention, the parameters of the gas chromatography-mass spectrometer preferably include: the temperature of the column box is 80 ℃, the temperature of the injection port is 280 ℃, and split-flow injection is not carried out. Temperature gradient: the initial temperature is 80 ℃, the temperature is kept for 1min, the temperature is raised to 220 ℃ at the rate of 20 ℃/min, the temperature is raised to 300 ℃ at the rate of 5 ℃/min, and the temperature is kept for 5 min.
In the present invention, the polycyclic aromatic hydrocarbon preferably includes naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, benzo [ a]Anthracene,
Benzo [ b ]]Fluoranthene, benzo [ k ]]Fluoranthene, benzo [ a ]]Pyrene, indene benzene [1,2,3-cd]Pyrene, dibenzo [ a, h ]]Anthracene and benzo [ g, h, i ]]One or more of perylene.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Mixing lean pork with pork fat (w: 8:2), making into meat patty, electrically baking for 12min, turning over every 2min to obtain blank meat sample, and applying to benzo [ a ═ a-]Anthracene,
Benzo [ b ]]Fluoranthene, benzo [ k ]]Fluoranthene, benzo [ a ]]Pyrene, indene benzene [1,2,3-cd]Pyrene, dibenzo [ a, h ]]Anthracene and benzo [ g, h, i ]]And (4) calibrating the perylene.
And ultrasonically extracting the blank meat sample by using normal hexane to obtain a purified blank meat sample, and using the purified blank meat sample for calibrating naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene and pyrene.
Adding 18 kinds of polycyclic aromatic hydrocarbon mixed standard solution into a blank meat sample, then stirring into minced meat, weighing 5g of minced meat, adding into a mortar, then adding 5g of anhydrous sodium sulfate and 5g of LC-Florisil diatomite, fully grinding, pouring into a 50mL polytetrafluoroethylene centrifugal tube, adding 20mL of mixed solvent of n-hexane and dichloromethane with the volume ratio of 1:1, whirling for 30s, placing the centrifugal tube into a centrifugal machine, centrifuging at the temperature of minus 4 ℃ at the rotating speed of 4500r/min for 10min, and taking supernatant; adding 20mL of mixed solvent of n-hexane and dichloromethane with the volume ratio of 1:1 into filter residue again, extracting under the same condition, centrifuging and filtering, combining the two filtered supernatants, placing in a rotary evaporator, performing rotary evaporation and concentration at 38 ℃ until the supernatant is nearly dry, and adding 5mL of n-hexane for re-dissolving to obtain a solution to be purified;
the method comprises the steps of activating the polycyclic aromatic hydrocarbon molecular imprinting column by using 5mL of n-hexane, balancing by using 5mL of dichloromethane, sampling 5mL of liquid to be purified after flowing and cleaning, adding the liquid to the polycyclic aromatic hydrocarbon molecular imprinting column, and eluting by using 10mL of dichloromethane as an eluent to obtain eluent and collecting the eluent. Placing the eluent in a nitrogen concentrator for concentration and constant volume to 0.5mL to obtain a sample to be detected;
the analysis parameters of the gas chromatography-mass spectrometer are set as follows:
the temperature of the column box is 80 ℃, the temperature of the sample inlet is 280 ℃, and the split-flow sample injection is not carried out.
The temperature gradient is that the initial temperature is 80 ℃, the temperature is kept for 1min, the temperature is raised to 220 ℃ at the rate of 20 ℃/min, the temperature is raised to 300 ℃ at the rate of 5 ℃/min, and the temperature is kept for 5 min.
Performing gas chromatography-mass spectrometry on a sample to be detected according to the chromatographic conditions, and determining the concentration when the signal-to-noise ratio (S/N) is 10 as a method quantification limit to obtain the linear concentration range and the quantification limit of the 18 polycyclic aromatic hydrocarbons, wherein the ranges and the quantification limits are shown in table 1. As can be seen from Table 1, figure 1 and figure 2, when the meat-containing sample prepared by the purification method provided by the invention is detected by a gas chromatography-mass spectrometry method, the content of impurities in the sample to be detected is small, the matrix effect is small, the interference of the impurities is not easy to occur when GC/MS detection is carried out, the reliability is high, the detection quantitative limit is low, and the contents of 18 polycyclic aromatic hydrocarbons in meat products can be detected simultaneously.
TABLE 1 Linear concentration ranges and quantitation limits for 18 polycyclic aromatic hydrocarbons obtained in example 1
Example 2
Mincing a preserved meat product into minced meat, weighing 5g of minced meat, adding the minced meat into a mortar, then adding 5g of anhydrous sodium sulfate and 5g of LC-Florisil diatomite, fully grinding, pouring into a 50mL polytetrafluoroethylene centrifugal tube, adding 20mL of mixed solvent of n-hexane and dichloromethane in a volume ratio of 1:1, swirling for 30s, placing the centrifugal tube into a centrifugal machine, centrifuging for 10min at the temperature of minus 4 ℃ at the rotating speed of 4500r/min, and taking supernatant; adding 20mL of mixed solvent of n-hexane and dichloromethane with the volume ratio of 1:1 into filter residue again, extracting under the same condition, centrifuging and filtering, combining the two filtered supernatants, placing in a rotary evaporator, performing rotary evaporation and concentration at 38 ℃ until the supernatant is nearly dry, and adding 5mL of n-hexane for re-dissolving to obtain a solution to be purified;
the method comprises the steps of activating the polycyclic aromatic hydrocarbon molecular imprinting column by using 5mL of n-hexane, balancing by using 5mL of dichloromethane, sampling 5mL of liquid to be purified after flowing and cleaning, adding the liquid to the polycyclic aromatic hydrocarbon molecular imprinting column, and eluting by using 10mL of dichloromethane as an eluent to obtain eluent and collecting the eluent. Concentrating the eluent in a nitrogen concentrator to be less than 0.5mL, adding an instrument internal standard, and then fixing the volume to be 0.5mL to obtain a sample to be detected;
the analysis parameters of the gas chromatography-mass spectrometer are set as follows:
the temperature of the column box is 80 ℃, the temperature of the sample inlet is 280 ℃, and the split-flow sample injection is not carried out.
The temperature gradient is that the initial temperature is 80 ℃, the temperature is kept for 1min, the temperature is raised to 220 ℃ at the rate of 20 ℃/min, the temperature is raised to 300 ℃ at the rate of 5 ℃/min, and the temperature is kept for 5 min.
And (3) carrying out gas chromatography-mass spectrometry on the sample to be detected according to the chromatographic conditions, and quantifying by using an internal standard curve method to obtain the preserved meat product, wherein the specific content range of the 18 polycyclic aromatic hydrocarbons is NQ (quantitative limit) -4.04 mu g/kg.
Example 3
The preparation method of the sample to be detected is the same as that in the embodiment 1, and the solvent is replaced by acetonitrile before detection;
detecting by adopting a liquid chromatogram-fluorescence detector, wherein the analysis parameters of the liquid chromatogram-fluorescence detector are set as follows: c18 liquid chromatography column, mobile phase: acetonitrile and water, polycyclic aromatic hydrocarbon excitation wavelength and emission wavelength are shown in table 2.
The concentration at which the signal-to-noise ratio (S/N) ═ 10 was determined as the quantitative limit of the method, and the linear concentration ranges and quantitative limits of the 15 polycyclic aromatic hydrocarbons obtained were as shown in table 2. As can be seen from Table 2, when the meat-containing sample prepared by the purification method provided by the invention is detected by a liquid chromatography-fluorescence detection method, the content of impurities in the sample to be detected is small, HPLC-FLD detection is carried out, the matrix effect is small, the interference of impurities is not easy to occur, the reliability is high, the detection quantitative limit is low, and the contents of 15 kinds of polycyclic aromatic hydrocarbons in meat products can be detected simultaneously.
Table 2 excitation wavelengths, emission wavelengths and resulting quantitation limits for 15 polycyclic aromatic hydrocarbons of example 3
Example 4
The preparation method of the sample to be detected is the same as that in the embodiment 2, and the solvent is replaced by acetonitrile before detection;
detecting a sample to be detected by adopting the detection method of the embodiment 3; and quantifying by an internal standard curve method to obtain the specific contents of the 15 polycyclic aromatic hydrocarbons in the meat product.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A method for purifying polycyclic aromatic hydrocarbon in a meat-containing sample is characterized by comprising the following steps:
mixing and grinding a meat-containing sample and chromatographically pure diatomite to obtain a ground material, wherein the meat-containing sample comprises meat and/or meat products;
mixing and extracting the ground material and an organic extraction solvent, wherein an extracted organic phase is a crude polycyclic aromatic hydrocarbon product, and the organic extraction solvent comprises dichloromethane or a mixed solvent of dichloromethane and n-hexane;
and purifying the crude polycyclic aromatic hydrocarbon by using a polycyclic aromatic hydrocarbon molecularly imprinted column, wherein the purified eluent comprises dichloromethane.
2. The purification method according to claim 1, wherein the mass ratio of the meat-containing sample to the chromatographically pure diatomaceous earth is not more than 1: 1.
3. The purification method according to claim 1 or 2, wherein the mixed ground raw material further comprises a solid desiccant, and the mass ratio of the solid desiccant to the diatomaceous earth is preferably 1: 1.
4. The purification method according to claim 1, wherein the volume ratio of dichloromethane to n-hexane in the mixed solvent of dichloromethane and n-hexane is not less than 0.5: 1.
5. The purification method according to claim 1, wherein the number of the mixed extraction is 2-3, and the volume ratio of the mass of the ground material to the volume of the organic extraction solvent is 5g:20 mL.
6. The purification method according to claim 1 or 5, wherein the mixed extraction is carried out under the condition of vortex oscillation, and the time of the vortex oscillation is 30s for each mixed extraction.
7. The purification method according to claim 5, wherein an extraction suspension is obtained after each mixing extraction, and after the mixing extraction, the method further comprises sequentially performing solid-liquid separation on the extraction suspension to obtain an extraction organic phase, combining the extraction organic phases, and concentrating to obtain the crude polycyclic aromatic hydrocarbon product, wherein the solid-liquid separation is centrifugation, the rotation speed of the centrifugation is 4500r/min, the centrifugation time is 10min, and the temperature of the extraction suspension is-20 to normal temperature during the centrifugation.
8. The purification method according to claim 7, wherein the concentration is rotary evaporation concentration, and the temperature of the concentration is 36-40 ℃.
9. A method for detecting polycyclic aromatic hydrocarbons in a meat-containing sample is characterized in that the purified meat-containing sample is detected by adopting a gas chromatography-mass spectrometry method or a high performance liquid chromatography-fluorescence detection method, and the purified meat-containing sample is obtained by the purification method of any one of claims 1 to 8.
10. The detection method according to claim 9, wherein the polycyclic aromatic hydrocarbon includes naphthalene, 1-methylnaphthalene, 2-methylnaphthalene, acenaphthylene, fluorene, phenanthrene, anthracene, fluoranthene, pyrene, perylene,Benzo [ a ]]Anthracene,
Benzo [ b ]]Fluoranthene, benzo [ k ]]Fluoranthene, benzo [ a ]]Pyrene, indene benzene [1,2,3-cd]Pyrene, dibenzo [ a, h ]]Anthracene and benzo [ g, h, i ]]One or more of perylene.
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