CN108414652B - Method for detecting content of anthracene and anthraquinone and anthrone oxides thereof in multi-medium environment - Google Patents
Method for detecting content of anthracene and anthraquinone and anthrone oxides thereof in multi-medium environment Download PDFInfo
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Abstract
The invention relates to a method for detecting the content of anthracene and anthraquinone and anthrone oxides thereof in a multi-medium environment. The method comprises the following steps: (1) pretreating a sample; (2) detecting by an instrument; the measuring method adopts GC-MS/MS to measure the content of anthracene, anthraquinone and anthrone in air, soil and water, has simple operation, and meets the requirements of environmental monitoring on detection limit, recovery rate, precision and the like.
Description
Technical Field
The invention relates to the technical field of polycyclic aromatic hydrocarbon compound detection, and particularly relates to a method for detecting the content of anthracene and anthraquinone and anthrone oxides thereof in a multi-medium environment.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) compounds are a class of persistent organic pollutants commonly existing in the environment and have the functions of carcinogenesis, teratogenesis and mutagenesis. In the growth process of crops, PAHs from multiple media such as air, soil, water and the like can be enriched, thereby causing the problem of food quality safety and bringing threat to human health. Anthracene (Anthracene ANT, CAS No 120-12-7, C)14H10) The PAHs is widely applied to industries such as dye, paper pulp and the like, is mainly produced by petroleum, coal and other fossil fuels and solid wastes such as wood, tobacco and the like in an incomplete combustion process, and is one of the prior pollutants of 16 PAHs confirmed by the United states environmental protection agency; the major oxidation product of AN is Anthraquinone (Anthraquinone AQ, CAS No 84-65-1, C)14H8O2) And Anthrone (Anthrone AT, CAS No 90-44-8, C)14H10O), among which AQ has reduced toxicity compared to ANT, but is also classified as a class 2B carcinogen by the world health organization international agency for research on cancer. AT present, no method for detecting ANT and oxidation products AQ and AT thereof in the environment is reported.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to design and provide a technical scheme of a method for detecting the content of anthracene and anthraquinone and anthrone oxide thereof in a multi-medium environment, and the method can provide technical support for AN source, conversion, bioremediation and the like in the environment.
The method for detecting the content of anthracene and anthraquinone and anthrone oxides thereof in the multi-medium environment is characterized by comprising the following steps:
1) sample pretreatment
Air: taking an air sample, and mixing the air sample with dichloromethane and acetone in a volume ratio of 4: 1, performing ultrasonic extraction for 3 times, combining all supernatants, performing concentration to a constant volume, and performing GC-MS/MS analysis;
soil: taking a soil sample, wherein the volume ratio of dichloromethane to acetone is 1: 1, performing vortex oscillation-ultrasonic extraction, centrifuging, taking supernatant, concentrating to constant volume, and performing GC-MS/MS analysis;
water: taking a water sample, distributing and extracting the water sample by using dichloromethane liquid, combining filtrate, concentrating to constant volume without purification, and performing GC-MS/MS analysis;
2) instrumental detection
Injecting sample into the standard working solution and the sample solution under the following set GC-MS/MS parameter conditions;
mass spectrum parameters:
the instrument condition parameters are as follows:
a chromatographic column: agilent J & W GC VF-5 ms; an ionization mode: EI; electron energy: 70 eV; ion source temperature: at 210 ℃; interface temperature: 280 ℃; sample inlet temperature: 250 ℃; procedure column temperature: the initial temperature is 80 ℃, the temperature is increased to 240 ℃ at 15 ℃/min, then the temperature is increased to 280 ℃ at 25 ℃/min, and the temperature is kept for 5 min. Carrier gas: 99.999% of helium and the flow rate is 1.0 mL/min; collision gas including argon 99.999% and 2.0 mTorr; sample introduction amount: 1 mu L of the solution; the sample feeding mode does not split;
the measurement method comprises the following steps: reaction monitoring mode was chosen, the maximum allowable deviation from ion abundance in qualitative confirmation: relative ion abundance > 50%, allowable relative deviation ± 20%; the relative ion abundance is more than 20-50%, and the allowable relative deviation is +/-25%; the relative ion abundance is more than 10-20%, and the allowable relative deviation is +/-30%; the relative ion abundance is less than or equal to 10 percent, and the allowable relative deviation is +/-50 percent;
3) blank test
The operation steps of the step 1) and the step 2) are carried out except that no sample is added;
4) result analysis and calculation
Drawing a 5-point standard working curve by taking the mass concentration as a horizontal coordinate X and the peak area ratio as a vertical coordinate Y, and quantifying a sample by using the standard working curve, wherein the response value of the medicine in the sample solution is in a linear range detected by an instrument; under the chromatographic conditions, whether the corresponding detected object exists in the sample or not is judged, and the following conditions are required to be met: the retention time of a mass spectrum chromatographic peak appearing in the sample solution is consistent with that of the standard substance working solution, the allowable deviation is less than +/-0.5%, the relative abundance of the drug corresponding to the chromatographic peak in mass spectrum qualitative ions is consistent with that of the mixed matrix standard working solution with the equivalent concentration, and the deviation of the relative abundance does not exceed the specification, so that the drug can be determined to be contained;
and calculating the content of anthraquinone in the sample by using chromatographic software or according to the following formula, wherein blank is required to be deducted from the calculation result:
in the formula:X i the residual quantity of the component i in the sample is mg/kg;
As: peak areas of i component drugs in the sample;
Asi: peak areas of i-component drugs in the standard sample;
Csi: the content of the i component medicament in the standard sample is ng/mu L;
Cf: a correction factor;
V 1 : sample amount of standard sample, μ L;
V 2 : the total volume of the extracting solution is mL;
V 3 : dividing the volume of the extracting solution to be mL;
V 4 : the volume of the sample is determined to be mL;
V 5 : sample size, μ L;
m: mass of sample, g.
The method for detecting the content of anthracene, anthraquinone oxide thereof and anthrone thereof in the multi-medium environment is characterized in that the pretreatment of an air sample specifically comprises the following steps: taking a glass fiber membrane, and carrying out a reaction on the glass fiber membrane by using 15mL of dichloromethane and acetone in a volume ratio of 4: 1 for 30min, extracting for 3 times according to the solution, merging all supernatants, carrying out rotary evaporation in a water bath at 35 ℃ until the supernatant is nearly dry, carrying out constant volume to 1mL by using a mixed solution of 0.04 mg/L anthraquinone-d8 n-hexane and acetone in a volume ratio of 39:1, filtering by using a 0.22 mu m filter membrane, and carrying out GC-MS/MS analysis.
The method for detecting the content of anthracene, anthraquinone oxide thereof and anthrone thereof in the multi-medium environment is characterized in that the soil sample pretreatment specifically comprises the following steps: taking a 2 g soil sample in a 50 mL polytetrafluoroethylene centrifuge tube, adding 20 mL dichloromethane: the volume ratio of acetone is 1: 1, performing ultrasonic extraction for 30min by vortex oscillation for 1 min, adding 1g of anhydrous magnesium sulfate, shaking up, cooling, performing vortex oscillation for 30 s, centrifuging for 5 min at 6000 r/min, taking 10 mL of supernatant, performing rotary evaporation at 35 ℃ in a heart bottle until the supernatant is nearly dry, performing constant volume to 1mL by using a mixed solution of anthraquinone-d8 n-hexane and acetone with the volume ratio of 39:1, filtering by a 0.22 mu m filter membrane, and performing GC-MS/MS analysis.
The method for detecting the content of the anthracene and the anthraquinone and anthrone oxides thereof in the multi-medium environment is characterized in that the pretreatment of a water sample specifically comprises the following steps: adding 100mL of water sample into a 250 mL separating funnel, adding 25 mL of dichloromethane, shaking up, performing liquid-liquid extraction for 2 times, combining lower-layer liquid, performing rotary evaporation in a water bath at 35 ℃ until the lower-layer liquid is nearly dry, performing constant volume to 1mL by using a mixed solution of 0.04 mg/L anthraquinone-d8 n-hexane and acetone in a volume ratio of 39:1, and filtering the mixed solution through a 0.22 mu m filter membrane to be analyzed by GC-MS/MS.
The invention develops GC-MS/MS in a multi-environment medium for the first time to simultaneously determine anthracene and metabolites thereof, namely anthraquinone and anthrone, and fills the technical blank. In addition, the invention provides the optimal conditions for determining anthracene, anthraquinone and anthrone in the environmental sample by the GC-MS/MS method.
Drawings
The compound of the structural formula shown in the figure 1 (A anthracene, B anthraquinone, C anthrone and D anthraquinone-D8 in sequence from left to right);
FIG. 2 is a mass spectrum of an air sample (blank, substrate plus-20 ppb in order from left to right);
FIG. 3 is a mass spectrum of a soil sample (blank, substrate plus-100 ppb in order from left to right);
FIG. 4 is a mass spectrum of a water sample (blank, matrix plus-10 ppb in order from left to right);
in FIGS. 2-4, A is anthracene, B is anthraquinone, C is anthrone, and D is anthraquinone-D8.
Detailed Description
The present invention is further illustrated by the following examples.
Examples
1. Reagents and materials
1.1 the normal hexane, the acetone and the dichloromethane are all chromatographic grades; anthracene, Anthraquinone, Anthrone, Anthraquinone-D8 standard substances (Anthracene CAS:120-12-7, Anthraquinone CAS:84-65-1, Anthraquinone CAS:90-44-8, Anthraquinone-D8 CAS: 10439-39-1): the purity is more than or equal to 99 percent.
1.2 standard stock solutions: accurately weighing a proper amount of standard substance (1.1), preparing 0.4mg/mL single-standard stock solution by using acetone, storing in a refrigerator at 0-4 ℃ in a dark place, and prolonging the effective period for 6 months.
1.3 preparation of standard working solution: diluting the standard stock solution (1.2) with acetone to obtain standard working solution with appropriate concentration, storing in 0-4 deg.C refrigerator in dark place, and prolonging the shelf life by 6 months.
1.4 microporous filter membrane: 0.22 μm, organic phase type.
2. Apparatus and device
GC-MS/MS (EI ion source); analytical balances (0.0001 g and 0.01g precision); a vortex mixer; a homogenizer; an oscillator; a height centrifuge; a rotary evaporator; a pulverizer. An ultrasonic cleaning machine; low-temperature cooling liquid circulating pump.
3. Measurement procedure
3.1 sample pretreatment
Air: one half of the glass fiber membrane was cut, and the cut half was washed with 15mL of dichloromethane: ultrasonically soaking in acetone (4: 1) for 30min, extracting for 3 times, mixing all supernatants, rotary evaporating at 35 deg.C in water bath to near dryness, adding 0.04 mg/L anthraquinone-d8 n-hexane: acetone (39: 1) was made up to 1mL and passed through a 0.22 μm filter (without purification) for GC-MS/MS analysis.
Soil: 2 g of sample was placed in a 50 mL Teflon centrifuge tube, and 20 mL of methylene chloride was added: extracting with acetone (1: 1) by ultrasonic wave for 30min under vortex oscillation for 1 min, adding 1g anhydrous magnesium sulfate, shaking and cooling. Vortex for 30 s, centrifuge for 5 min at 6000 r/min, take 10 mL supernatant in the heart bottle 35 ℃ rotary evaporation to near dry, with anthraquinone-d8 n-hexane: acetone (39: 1) was made up to 1mL, filtered through a 0.22 μm filter (no purification required) and analyzed by GC-MS/MS.
Water: 100mL of water was put in a 250 mL separatory funnel, 25 mL of methylene chloride was added thereto, and the mixture was shaken up to conduct liquid-liquid extraction 2 times. Combining the lower layer liquid, carrying out rotary evaporation on the lower layer liquid in a water bath at 35 ℃ until the lower layer liquid is nearly dry, and carrying out reaction on the lower layer liquid by using anthraquinone-d8 n-hexane with the concentration of 0.04 mg/L: acetone (39: 1) was made up to 1mL and passed through a 0.22 μm filter (without purification) for GC-MS/MS analysis.
3.2 instrumental detection
Due to the differences in chromatographic conditions between different instrument models, the conditions provided below have proven suitable, with specific parameters in table 1 and mass spectral parameters in table 2.
TABLE 1 GC-MS/MS parameter conditions
TABLE 2 Mass Spectrometry parameters
Denotes quantitative ions
4. Blank test
The procedure was followed except that no sample was added.
5. Result analysis and calculation
Drawing a 5-point standard working curve by taking the mass concentration as a horizontal coordinate X and the peak area ratio as a vertical coordinate Y, and quantifying a sample by using the standard working curve, wherein the response value of the medicine in the sample solution is in a linear range detected by an instrument; under the chromatographic conditions, whether the corresponding detected object exists in the sample or not is judged, and the following conditions are required to be met: and the retention time of a mass spectrum chromatographic peak appearing in the sample solution is consistent with that of the standard working solution, the allowable deviation is less than +/-0.5%, the relative abundance of the drug corresponding to the chromatographic peak in mass spectrum qualitative ions is consistent with that of the mixed matrix standard working solution with the equivalent concentration, and the deviation of the relative abundance does not exceed the specification, so that the drug can be determined to be contained.
Calculating the anthraquinone content in the sample by using chromatographic software or according to the following formula, wherein blank is required to be deducted from the calculation result:
in the formula:X i the residual quantity of the component i in the sample is mg/kg;
As: peak areas of i component drugs in the sample;
Asi: peak areas of i-component drugs in the standard sample;
Csi: the content of the i component medicament in the standard sample is ng/mu L;
Cf: a correction factor;
V 1 : sample amount of standard sample, μ L;
V 2 : the total volume of the extracting solution is mL;
V 3 : dividing the volume of the extracting solution to be mL;
V 4 : the volume of the sample is determined to be mL;
V 5 : sample size, μ L;
m: mass of sample, g.
6. Minimum limit of detection
The determination lower limit of the method is 0.2 mu g/kg.
7. Recovery rate
In the method, three addition concentrations are set in the recovery rate test, 3 times of experiments are carried out on each addition concentration according to the experimental conditions determined by the method in the embodiment, the results of the recovery rate and the precision are shown in table 3, and mass spectrograms of an air sample, a soil sample and a water sample are shown in fig. 2-4.
TABLE 3 sample addition concentration and recovery Range
Claims (1)
1. The method for detecting the content of anthracene, anthraquinone oxide thereof and anthrone thereof in a multi-medium environment is characterized by comprising the following steps:
1) sample pretreatment
Air: taking a glass fiber membrane, and carrying out a reaction on the glass fiber membrane by using 15mL of dichloromethane and acetone in a volume ratio of 4: 1 for 30min, extracting for 3 times in the mode, combining all supernatants, carrying out rotary evaporation in a water bath at 35 ℃ until the supernatants are nearly dry, carrying out constant volume to 1mL by using a mixed solution with the concentration of 0.04 mg/L anthraquinone-d8 n-hexane and acetone in the volume ratio of 39:1, and filtering the mixed solution through a 0.22 mu m filter membrane for GC-MS/MS analysis;
soil: taking a 2 g soil sample in a 50 mL polytetrafluoroethylene centrifuge tube, adding 20 mL dichloromethane: the volume ratio of acetone is 1: 1, performing ultrasonic extraction for 30min by vortex oscillation for 1 min, adding 1g of anhydrous magnesium sulfate, shaking up, cooling, performing vortex oscillation for 30 s, centrifuging for 5 min at 6000 r/min, taking 10 mL of supernatant, performing rotary evaporation at 35 ℃ in a heart bottle until the supernatant is nearly dry, performing constant volume to 1mL by using a mixed solution of anthraquinone-d8 n-hexane and acetone with the volume ratio of 39:1, filtering by a 0.22 mu m filter membrane, and performing GC-MS/MS analysis;
water: taking 100mL of water sample into a 250 mL separating funnel, adding 25 mL of dichloromethane, shaking up for liquid-liquid extraction for 2 times, combining lower-layer liquid, carrying out rotary evaporation in a water bath at 35 ℃ until the lower-layer liquid is nearly dry, carrying out constant volume to 1mL by using a mixed solution with the concentration of 0.04 mg/L anthraquinone-d8 n-hexane and acetone in the volume ratio of 39:1, filtering the mixed solution by a 0.22 mu m filter membrane, and carrying out GC-MS/MS analysis;
2) instrumental detection
Injecting sample into the standard working solution and the sample solution under the following set GC-MS/MS parameter conditions;
mass spectrum parameters:
the instrument condition parameters are as follows:
a chromatographic column: agilent J & W GC VF-5 ms; an ionization mode: EI; electron energy: 70 eV; ion source temperature: at 210 ℃; interface temperature: 280 ℃; sample inlet temperature: 250 ℃; procedure column temperature: the initial temperature is 80 ℃, the temperature is increased to 240 ℃ at the speed of 15 ℃/min, then the temperature is increased to 280 ℃ at the speed of 25 ℃/min, and the temperature is kept for 5 min; carrier gas: 99.999% of helium and the flow rate is 1.0 mL/min; collision gas including argon 99.999% and 2.0 mTorr; sample introduction amount: 1 mu L of the solution; the sample feeding mode does not split;
the measurement method comprises the following steps:
reaction monitoring mode was chosen, the maximum allowable deviation from ion abundance in qualitative confirmation: relative ion abundance > 50%, allowable relative deviation ± 20%; the relative ion abundance is 20-50%, and the allowable relative deviation is +/-25%; the relative ion abundance is 10-20%, and the allowable relative deviation is +/-30%; the relative ion abundance is less than or equal to 10 percent, and the allowable relative deviation is +/-50 percent;
3) blank test
The operation steps of the step 1) and the step 2) are carried out except that no sample is added;
4) result analysis and calculation
Drawing a 5-point standard working curve by taking the mass concentration as a horizontal coordinate X and the peak area ratio as a vertical coordinate Y, and quantifying a sample by using the standard working curve, wherein the response value of the medicine in the sample solution is in a linear range detected by an instrument; under the chromatographic conditions, whether the corresponding detected object exists in the sample or not is judged, and whether the following conditions are met or not is judged: the retention time of a mass spectrum chromatographic peak appearing in the sample solution is consistent with that of a standard working solution, the allowable deviation is less than +/-0.5%, the relative abundance of the drug corresponding to the chromatographic peak in mass spectrum qualitative ions is consistent with that of the mixed matrix standard working solution with the equivalent concentration, and the relative abundance deviation does not exceed the specification, namely the maximum allowable deviation of the relative ion abundance during qualitative confirmation: relative ion abundance > 50%, allowable relative deviation ± 20%; the relative ion abundance is 20-50%, and the allowable relative deviation is +/-25%; the relative ion abundance is 10-20%, and the allowable relative deviation is +/-30%; the abundance of the relative ions is less than or equal to 10 percent, and the allowable relative deviation is +/-50 percent, so that the medicine can be determined to be contained;
and calculating the content of anthraquinone in the sample by using chromatographic software or according to the following formula, and deducting blank from the calculation result:
in the formula:X i the residual quantity of the component i in the sample is mg/kg;
As: peak areas of i component drugs in the sample;
Asi: peak areas of i-component drugs in the standard sample;
Csi: the content of the i component medicament in the standard sample is ng/mu L;
Cf: a correction factor;
V 1 : sample amount of standard sample, μ L;
V 2 : the total volume of the extracting solution is mL;
V 3 : dividing the volume of the extracting solution to be mL;
V 4 : the volume of the sample is determined to be mL;
V 5 : sample size, μ L;
m: mass of sample, g.
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