LU102485B1 - Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water - Google Patents
Method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water Download PDFInfo
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- LU102485B1 LU102485B1 LU102485A LU102485A LU102485B1 LU 102485 B1 LU102485 B1 LU 102485B1 LU 102485 A LU102485 A LU 102485A LU 102485 A LU102485 A LU 102485A LU 102485 B1 LU102485 B1 LU 102485B1
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- aromatic hydrocarbons
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 238000000034 method Methods 0.000 title claims abstract description 46
- 238000004458 analytical method Methods 0.000 title claims abstract description 31
- 238000000605 extraction Methods 0.000 title claims abstract description 29
- 125000005575 polycyclic aromatic hydrocarbon group Chemical group 0.000 title claims abstract description 24
- 239000012528 membrane Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 238000001514 detection method Methods 0.000 claims abstract description 13
- 239000007790 solid phase Substances 0.000 claims abstract description 11
- 238000004949 mass spectrometry Methods 0.000 claims abstract description 7
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 57
- GVEPBJHOBDJJJI-UHFFFAOYSA-N fluoranthene Chemical compound C1=CC(C2=CC=CC=C22)=C3C2=CC=CC3=C1 GVEPBJHOBDJJJI-UHFFFAOYSA-N 0.000 claims description 37
- BBEAQIROQSPTKN-UHFFFAOYSA-N pyrene Chemical compound C1=CC=C2C=CC3=CC=CC4=CC=C1C2=C43 BBEAQIROQSPTKN-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 19
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 claims description 14
- MWPLVEDNUUSJAV-UHFFFAOYSA-N anthracene Chemical compound C1=CC=CC2=CC3=CC=CC=C3C=C21 MWPLVEDNUUSJAV-UHFFFAOYSA-N 0.000 claims description 14
- YNPNZTXNASCQKK-UHFFFAOYSA-N phenanthrene Chemical compound C1=CC=C2C3=CC=CC=C3C=CC2=C1 YNPNZTXNASCQKK-UHFFFAOYSA-N 0.000 claims description 14
- 239000011550 stock solution Substances 0.000 claims description 13
- HXGDTGSAIMULJN-UHFFFAOYSA-N acetnaphthylene Natural products C1=CC(C=C2)=C3C2=CC=CC3=C1 HXGDTGSAIMULJN-UHFFFAOYSA-N 0.000 claims description 12
- NIHNNTQXNPWCJQ-UHFFFAOYSA-N fluorene Chemical compound C1=CC=C2CC3=CC=CC=C3C2=C1 NIHNNTQXNPWCJQ-UHFFFAOYSA-N 0.000 claims description 12
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 claims description 11
- CWRYPZZKDGJXCA-UHFFFAOYSA-N acenaphthene Chemical compound C1=CC(CC2)=C3C2=CC=CC3=C1 CWRYPZZKDGJXCA-UHFFFAOYSA-N 0.000 claims description 10
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 10
- 239000003085 diluting agent Substances 0.000 claims description 9
- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 claims description 7
- 239000012086 standard solution Substances 0.000 claims description 7
- 125000004054 acenaphthylenyl group Chemical group C1(=CC2=CC=CC3=CC=CC1=C23)* 0.000 claims description 6
- 125000005605 benzo group Chemical group 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000001195 ultra high performance liquid chromatography Methods 0.000 claims description 6
- 238000010828 elution Methods 0.000 claims description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 5
- 239000010931 gold Substances 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 5
- 238000002347 injection Methods 0.000 claims description 5
- 239000007924 injection Substances 0.000 claims description 5
- 239000012071 phase Substances 0.000 claims description 5
- 238000000611 regression analysis Methods 0.000 claims description 5
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical group O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 claims description 5
- 238000007865 diluting Methods 0.000 claims description 4
- 241001421757 Arcas Species 0.000 claims description 3
- 201000003639 autosomal recessive cerebellar ataxia Diseases 0.000 claims description 3
- 238000003795 desorption Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 230000010355 oscillation Effects 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 claims description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 46
- 150000002500 ions Chemical class 0.000 description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000874 microwave-assisted extraction Methods 0.000 description 2
- 238000000899 pressurised-fluid extraction Methods 0.000 description 2
- 238000002470 solid-phase micro-extraction Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- TXVHTIQJNYSSKO-UHFFFAOYSA-N BeP Natural products C1=CC=C2C3=CC=CC=C3C3=CC=CC4=CC=C1C2=C34 TXVHTIQJNYSSKO-UHFFFAOYSA-N 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- FTOVXSOBNPWTSH-UHFFFAOYSA-N benzo[b]fluoranthene Chemical compound C12=CC=CC=C1C1=CC3=CC=CC=C3C3=C1C2=CC=C3 FTOVXSOBNPWTSH-UHFFFAOYSA-N 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 238000001294 liquid chromatography-tandem mass spectrometry Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- VLCQZHSMCYCDJL-UHFFFAOYSA-N tribenuron methyl Chemical compound COC(=O)C1=CC=CC=C1S(=O)(=O)NC(=O)N(C)C1=NC(C)=NC(OC)=N1 VLCQZHSMCYCDJL-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Classifications
-
- 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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1826—Organic contamination in water
-
- 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
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
- G01N2030/8854—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds involving hydrocarbons
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The disclosure relates to a method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water. A parallel solid-phase membrane sheet sample pretreatment microplate system device involved in this method is composed of an oscillating device, a sample container and a membrane sheet system. An ultra-high performance liquid chromatography-triple quadrupole rod mass spectrometry is used to quantitatively determine the content of environmental pollutant polycyclic aromatic hydrocarbons, wherein the detection is completed within 10 min, and the average pretreatment time of each sample is about 1 min. This method is good in reproducibility and stability, and is a rapid and effective means to extract and determine the content of polycyclic aromatic hydrocarbons in water.
Description
BL-5187 METHOD FOR RAPID EXTRACTION AND ANALYSIS OF 10 U1 00485
[0001] This application claims priority to Chinese Patent Application No. 201910492469 .4 filed on June 6, 2019, the entire contents of which are incorporated herein by reference.
[0002] The disclosure relates to a method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water, in which a parallel solid-phase membrane sheet sample pretreatment microplate system device is utilized to rapidly extract samples. and a method for rapid analysis and determination in the content of polycyclic aromatic hydrocarbons in water using an ultra-high performance liquid chromatography- mass spectrography.
[0003] The environmental pollutants polycyclic aromatic hydrocarbons PAHs are compounds having two and more than two benzene rings, which are weak in polarity and easily dissolved into non-polar and moderate-polar solvents. Extraction methods of PAHs mainly include a Soxhlet extraction method. an ultrasonic extraction method. a microwave extraction method. an accelerated solvent extraction method and a solid phase micro-extraction method. The Soxhlet extraction method involves tedious operations is time-consuming and solvent-consuming: the microwave extraction method is not ideal in extraction efficiency of low-ring compounds; the accelerated solvent extraction method and the solid phase micro-extraction method need to configuration of instruments which are high in maintenance and use costs; regardless of which extraction method, it needs lots of samples, and is complicated in process.
[0004] Solvents for extracting PAHSs are mainly mixed solvents of dichloromethane, n-hexane and acetone in different ratios. Before liquid chromatographic analysis. it is needed to convert a solvent such as dichloromethane, n-hexane and acetone into acetonitrile, methanol or other solvents. however, the solvent conversion process involve steps of spin cvaporation. nitrogen blowing and the like. which are prone to causing loss of to-be-detected objects and insufficient solvent conversion.
[0005] Although the relevant document “SIMULTANEOUS DETERMINATION OF 16
POLYCYCLIC AROMATIC HYDROCARBONS RESIDUES IN ELECTRONIC AND ELECTRICAL PRODUCTS USING LIQUID CHROMATOGRAPHY- ATMOSPHERIC 1
BL-5187 PHOTOELECTRIC INIZATION SOURCE MASS SPECTROMETRY" (Juyi Yin, Donghua Xie, Jianguo Chen, etc.) uses HPLC-MS to detect polycyclic aromatic hydrocarbons, relative to this 102465 method, the extraction method in the above document is complicated and time-consuming and different in detected samples, and the disclosure is mainly directed to a method for detecting 10 polycyclic aromatic hydrocarbons in a water sample.
[0006] Relatively speaking. a parallel solid-phase membrane sheet sample pretreatment microplate system extraction method based on LC/MS/MS provided by the disclosure is convenient to operate, low in cost, small in sample amount and suitable for simultaneously treating samples on large scale. Meanwhile, the method provided by the disclosure has the advantages of short test time, good reproducibility and the like.
[0007] The object of the disclosure is to provide a method for rapid extraction and analysis of polycyclic aromatic hydrocarbons in water. The parallel solid-phase membrane sheet sample pretreatment microplate system device involved in this method is composed of a membrane sheet system 1. a 96-well plate 2 and an oscillating device 3. An ultra-high performance liquid chromatography-triple quadrupole rod mass spectrometry 18 used to quantitatively determine the content of environmental pollutants, 1.e., polycyclic aromatic hydrocarbons. The detection is completed within 10 min, and the average pretreatment time of each sample is about 1 min. This method is good in reproducibility and stability, and is a rapid and effective means to extract and determine the content of polycyclic aromatic hydrocarbons in water.
[0008] The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water provided by the disclosure comprises the following steps:
[0009] a. sample treatment: adding a water sample in a sample container, oscillating the sample container and meanwhile adsorbing the water sample for 50 min: taking a new sample container. adding a solution of acetonitrile and water in a volume ratio of 80:20 in the sample container. oscillating and desorbing for 50 min: and then injecting the water sample to an ultra-high performance liquid chromatograph- mass spectrograph for analysis and detection:
[0010] b. conditions of ultra-high performance liquid chromatography: mobile phase: A-water. and B-acetonitrile: elution gradient: 0-2 min, À 60%: 2-3 min. A 60%-20%: 3.0-8.0 min. A 20%:
8.0-8.1 min. A 20%-60%; 8.1-10.0 min. A 60%. flow rate: 0.35 ml./min: column temperature: 30°C: injection amount: 5 ul:
[0011] c. conditions of mass spectrometry: ion source current: +4.0v: ion source temperature: 2
BL-5187 400°C; sheath gas: 35 arb: auxiliary gas: 5 arb; ion transfer capillary tube temperature: 350°C: LU102485
[0012] d. preparation of control solution: precisely fetching 100 pl. of control, dissolving the control with acetonitrile into a constant volume of 1 mL as a control stock solution:
[0013] ©. plotting of standard curves: precisely fetching the control stock solution, respectively diluting the control stock solution into different concentrations with a diluent to obtain standard solutions: performing ultra-high performance liquid chromatography-mass spectrometry according to chromatographic conditions: and performing regression analysis by concentration versus area. so as to obtain standard component curves, and calculating regression equations: and
[0014] f. determination of contents: precisely sucking a sample to-be-detected solution. performing ultra-high performance liquid chromatography-mass spectrometry according to chromatographic conditions and introducing peak areas into the standard curves to calculate contents, so as to obtain detection results.
[0015] According to the method for rapid extraction and analysis of 10 polveyelic aromatic hydrocarbons in water provided by the disclosure. preferably. sample treatment adopts the parallel] solid-phase membrane sheet sample pretreatment microplate system device which is mainly composed of a membrane sheet system . a sample container and an oscillating device:
[0016] when in sample treatment. the water sample is added in the sample container. the sample container is placed in the oscillating device to be oscillated by the oscillating device and adsorption 1s conducted by the membrane sheet system. a new sample container is changed. acetonitrile and water being in a volume ratio of 80:20 are added in the sample container to perform oscillation and desorption for 50 min, and then the water sample is injected to an ultra- high performance liquid chromatograph-mass spectrograph for analysis and detection.
[0017] The membrane sheet system of the disclosure is mainly composed of a membrane sheet and a fixation frame for fixing the membrane sheet. The membrane sheet can adopt a stainless steel sheet having a thickness of 0.5-2 mm and a size of (1-10) x (20-80) mm (preferably. a thickness of 1 mm and a size of 5 x 50 mm). a coating is coated on the stainless steel sheet by virtue of a chemical bond and a physical means. so as to prepare a membrane-shaped extraction sheet having a certain coating thickness. The material coating the membrane can be. but is not limited to. DVB (divinyl benzene) or C18. Different coating material can be selected according to the detected samples. The thickness of the coated coating can be 0.3-2 mm. for example. but is not limited to. 0.5 m. 1 mm. 1.5 mm and 2 mm.
3
BL-5187
[0018] The oscillating device involved in the disclosure can be any oscillating device that can 02485 realize the disclosure and 1s conventional in the art. and cannot be defined specially here.
[0019] When the parallel solid-phase membrane sheet sample pretreatment microplate system device of the disclosure is operated. the sample container is directly clamped in the oscillating device and can be flexibly put in the oscillating device. the membrane sheet system is vertically immersed into the liquid inside the sample container to be adsorbed and eluted.
[0020] According to the method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water provided by the disclosure. preferably. in step b, and a chromatographic column for ultra-high performance liquid chromatography is Hypersil GOLD, C18 100 = 2.1 mm.
1.9 um or an equivalent column thereof.
[0021] According to the method for rapid extraction and analysis of 10 polyvevelic aromatic hydrocarbons in water provided by the disclosure. preferably. in step c. the ion source type is an atmospheric pressure chemical APCT ion source.
[0022] According to the method for rapid extraction and analysis of 10 polycyclie aromatic hydrocarbons in water provided by the disclosure, preferably. in step e. the diluent is a solution having a volume ratio of water to acetonitrile being 20:80.
[0023] According to the method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water provided by the disclosure. preferably. in step e. the used diluent is used to respectively perform dilution to form 2 ng/mL. 4 ng/mL. 20 ng/mL. 40 ng/mL. 200 ng/ml. and 400 ng/ml, so as to obtain standard solutions.
[0024] According to the method for rapid extraction and analysis of 10 polyevelic aromatic hydrocarbons in water provided by the disclosure. preferably. the sample container can be any container in the art, for example. but is not limited to. a perforated plate. further preferably. the sample container can be a 96-well plate.
[0025] According to the method for rapid extraction and analysis of 10 potveyelic aromatic hydrocarbons in water provided by the disclosure. as a preferred manner. the technical solution of the disclosure can be as follows:
[0026] Provided is a method for rapid extraction and analysis of 10 polveyelic aromatic hydrocarbons in water. the parallel solid-phase membrane sheet sample pretreatment microplate system device involved in the method is composed of an oscillating device 3. a 96-well plate 2 and a membrane sheet system |. and specific operations are performed as follows: 4
BL-5187
[0027] a, sample treatment: adding a water sample in a 96-well plate 2, placing the 96-well 92485 plate 2 in an oscillating device 3 10 be oscillated by the oscillating device 3 and meanwhile adsorbing the water sample with the membrane sheet system 1 for 30 min; taking a new 96-well plate 2. adding a solution of acetonitrile and water in a volume ratio of 80:20 in each well, oscillating and desorbing for 50 min. and then putting the 96-well plate 2 in an automatic sample injector lo inject the sample into an ultra-high performance liquid chromatograph-mass spectrograph for analysis and detection:
[0028] b. conditions of ultra-high performance liquid chromatography: chromatographic column: Hypersil GOLD. C18 100 x 2.1 mm. 1.9 um: mobile phase: A-water, and B-acetonitrile: elution gradient: 0-2 min. A 60%: 2-3 min. A 60%-20%: 3.0-8.0 min, A 20%; 8.0-8.1 min. A 20%- 60%: 8.1-10.0 min. À 60%, flow rate: 0.33ml./min: column temperature: 30°C: injection amount: ul:
[0029] c. conditions of mass spectrometry: ion source current: +4.0 v: ion source temperature: 400 ©: sheath gas: 35 arb: auxiliary gas: 5 arb; ion transfer capillary tube temperature: 350°C: ion source type: atmospheric chemical APCT ion source: {0030} d. preparation of control solution: precisely fetching 100 uL of control. dissolving the control with acetonitrile into a constant volume of 1 ml. as a control stock solution:
[0031] e. standard curve plotting: precisely fetching the control stock solution, respectively diluting the control stock solution into 2 ng/mL. 4 ng/ml.. 20 ng/mL. 40 ng/ml.. 200 ng/ml. and 400 ng/mL with a diluent to obtain standard solutions: performing ultra-high performance liquid chromatography-mass spectrometry according to chromatographic conditions: and performing regression analysis by concentration versus area. so as to obtain standard component curves, and calculating regression equations: and
[0032] f. determination of contents: precisely sucking a sample to-be-detected solution. performing ultra-high performance liquid chromatography-mass spectrometry according 10 chromatographic conditions and introducing peak arcas into the standard curves to calculate contents, wherein detection results are as follows: naphthalene 6.0-207 ng: accnaphthene 2.4-30.7 ng. acenaphthylene 1.7-48.0 ng: fluorene 5.6-60.5 ng: phenanthrene 11.1-64.2 ne: anthracene !.06-66.8 ne: fluoranthene 3.9-32.5 ne: pyrene 3.7-70.4 ne: benzopyrene b fluoranthene 1.7-16 ng: benzo a pyrene 18-118 ne.
[0033] Fig.l isaspectrogram of a standard sample according to the disclosure. in which peaks 5
BL-5187 of total ion current spectrums are as follows: naphthalene (4.15 min): acenaphthylene (4.30 min); . . . LU102485 fluorene (4.53 min); acenaphthene (4.54 min): phenanthrene (4.63 min); anthracene (4.72 min): fluoranthene (4.94 min); pyrene (5.09 min); benzo (b) fluoranthene (6.00 min); benzo (a) pyrene (6.22 min).
[0034] Fig.2 is a diagram of a parallel solid-phase membrane sheet sample pretreatment microplate system device according to the disclosure.
[0035] Examples
[0036] In the disclosure, a lab water sample is taken as an example, the prepared sample is extracted according to a preparation method provided by the disclosure, and the contents of polycyclic aromatic hydrocarbons are determined according to a determination method provided by the disclosure.
[0037] Instruments and reagents:
[0038] Ultra-high performance liquid chromatograph (Agilent 1290); mass spectrograph (Thermo TSQ QUANTUM ULTRA); ten-thousandth electronic balance (METTLER AM100); acetonitrile is a chromatographic pure reagent, and polycyclic aromatic hydrocarbon is control (BePure).
[0039] Instrument conditions:
[0040] Conditions of ultra-high performance liquid chromatograph:
[0041] Hypersil GOLD, Ci8 100 x 2.1 mm, 1.9 um; mobile phase: A-ultrapure water. B- acetonitrile; elution gradient: ~~ Time A% B% mi) 0 60 40 2 60 40 3 20 80 8 20 80
8.1 60 40
10.0 60 40
[0042] Flow rate: 0.35 ml/min: column temperature: 30 C: injection amount: 5 ul:
[0043] conditions of mass spectrograph: ion source current: +4.0 v: ion source temperature: 400 C: sheath gas: 35 arb: auxiliary gas: 5 arb: ion transfer capillary tube temperature: 350 C: jon source type: atmospheric chemical APCI ion source: Parent ions Son ions ; Lo
BL-5187 (QE m/z) Rwy LU102485 Naphthalene 128.198 77.168*: 78.247; 102.093 Acenaphthenc 153.138 126.006: 150.998+; 152.013 Acenaphthylene 153.138 126.006: 150.998; 152.013* Fluorine 165.116 115.077*: 162.994; 164.008 Phenanthrene 178.095 150.968: 151.971#; 175.97 Anthracene 178,095 150.968; 151.971; 175.97* Fluoranthene 202.057 150.991. 199.972*: 201.016 Pyrene 202.057 150,998; 199.972: 201.016* Benzopyrene b fluoranthene 252.018 225.868*; 249.932 Benzo a pyrene 252.018 225.868: 249.932%
[0044] Sample treatment: 2 mL of water sample was precisely sucked and placed in wells of a 96-well plate 2. the 96-well plate 2 was placed in a parallel solid-phase membrane sheet system to be oscillated by an oscillating device 3 and meanwhile the water sample was adsorbed with the membrane sheet system 1 for 50 min. a new 96-well plate 2 was used. a solution of acetonitrile and water in a volume ratio of 80:20 were added in cach well of the new 96-well plate 2. analyzed and desorbed for 50 min. and then the 96-well plate 2 was put in an automatic sample injector to inject the sample into an ultra-high performance liquid chromatograph-mass spectrograph for analysis:
[0045] Preparation of control solution: 100 pl. of control was precisely fetched and dissolved with acetonitrile into a constant volume of 1 mL as a control stock solution:
[0046] plotting of standard curves: the control stock solution was precisely fetched. and respectively diluted into 2 ng/mL. 4 ng/mL. 20 ng/ml. 40 ng/ml.. 200 ng/mL and 400 ng/ml. using a diluent namely a solution having a volume ratio of water to acetonitrile being 20:80 to obtain standard solutions: ultra-high performance liquid chromatography-mass spectrometry was performed according to chromatographic conditions: regression analysis was performed by concentration versus area. so as to obtain standard component curves. and regression equations were caleulated: naphthalene, Y=2178.29:67.6777*X. R-=0.9975. n76: acenaphthene Y-
4028.56-100.466*X. R°-0.99993, n--6: acenaphthylene. Y=6233.36+616.158#X. R7-0.9989. n°7: fluorene. Ÿ -3119.73+163.784*X, R°=0,9993, n=6: phenanthrene Y-6227. 19-286 401*X. 7
BL-5187 R=0.9982. n=8: anthracene Y=6399.69+593.228*X. R> 0.9988, n=7: fluoranthene , LU102485 Y=13232.8+501.493*X. R=0.9987, n=7: pyrene Y=10948.7+861.248*X, R°=0.9991, n=7; benzopyrene b fuoranthene Y=151.24712556.68*X. R°=0.9992, n=6; benzo a pyrene Y=- 23181+2382.35*X. R*=0.9987. n=6.
[0047] determination of contents: a to-be-detected sample solution was precisely sucked, ultra- high performance liquid chromatography-mass spectrometry was performed according to chromatographic conditions and peak arcas were introduced into the standard curves to calculate contents:
[0048] detection results of samples: naphthalene 6.0-207 ng: acenaphthene 2.4-30.7 ng: acenaphthylene 1.7-48.0 ng: fluorene 5.6-60.5 ng: phenanthrene 11.1-64.2 ng; anthracene 1.06-
66.8 ng: fluoranthene 5.9-52.5 ne: pyrene 3.7-70.4 ne: benzopvrene B fluoranthene 1.7-16 ne: benzo a pyrene 18-118 ne.
[0049] Repeatability test: 7 samples were taken. According to the steps. RSD results are as follows: naphthalene 4.19%; acenaphthene 4.01%: acenaphthvlene 3.98%: fluorene 1.55%: phenanthrene 6.19%: anthracene 4.6%: fluoranthene 4.82%: pyrene 5.33%: benzopyrene b fluoranthene 2.82%: benzo a pyrene 1.87%.
8
Claims (9)
1. A method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water, comprising the following steps: a, sample treatment: adding a water sample in a sample container, oscillating the sample container and meanwhile adsorbing the water sample for 50 min, taking a new sample container. adding a solution of acetonitrile and water in a volume ratio of 80:20 into the sample container, oscillating and desorbing for 50 min. and then injecting the water sample to an ultra-high performance liquid chromatograph- mass spectrograph for analysis and detection: b. conditions of ultra-high performance liquid chromatography: mobile phase: A-water, and B-acetonitrile: elution gradient: 0-2 min. A 60%: 2-3 min. À 60%-20%; 3.0-8.0 min, A 20%: 8.0-
8.1 min. A 20%-60%: 8.1-10.0 min. A 60%, flow rate: 0.35 mL/min; column temperature: 30°C: injection volume: 5 ul: c. conditions of mass spectrometry: ion source current: +4.0 v; ion source temperature: 400°C: sheath gas: 35 arb: auxiliary gas: 5 arb: ion transfer capillary tube temperature: 350°C: d. preparation of control solution: precisely fetching 100 pL of control, dissolving the control with acctonitrile into a constant volume of 1 mL as a control stock solution: e. plotting of standard curves: precisely fetching the control stock solution. respectively diluting into different concentrations with a diluent to obtain standard solutions: performing ultra- high performance liquid chromatography-mass spectrometry according to chromatographic conditions; and performing regression analysis by concentration versus peak area, so as to obtain standard component curves, and calculating regression equations: and {. determination of contents: precisely sucking a sample to-be-detected solution. performing ultra-high performance liquid chromatography-mass spectrometry according to chromatographic conditions and introducing peak arcas into the standard curves to calculate contents. so as to obtain detection results.
2. The method for rapid extraction and analysis of 10 polyeyelic aromatic hydrocarbons in water according to claim 1. wherein in the method. à parallel solid-phase membrane sheet sample pretreatment microplate system device is used for sample treatment. and the device is composed of a membrane sheet system. a sample container and an oscillating device: when m sample treatment, a water sample 1s added in the sample container. the sample container is placed in the oscillating device to be oscilluted by the oscillating device. adsorption 9
BL-5187 is performed by a membrane sheet system, a new sample container is changed. acetonitrile and . € . . oy LU102485 water having a volume ratio of 80:20 are added in the sample container to perform oscillation and desorption for 50 min. and then the water sample is injected to an ultra-high performance liquid chromatograph-mass spectrograph for analysis and detection.
3. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to claim 1 or 2, wherein in step b, and a chromatographic column for ultra-high performance liquid chromatography is Hypersil GOLD, Ci8 100 x 2.1 mm. 1.9 pm or an equivalent column thercof.
4. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to claim 1 or 2, wherein in step €. an ion source type is an atmospheric pressure chemical APCTion source.
3. The method for rapid extraction and analysis of 10 polyeyclie aromatic hydrocarbons in water according to claim | or 2, wherein in step e, the diluent is a solution having a volume ratio of water to acetonitrile being 20:80.
6. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to claim 1 or 2, wherein in step e. the diluent is used to respectively perform dilution to form 2 ng/mL. 4 ng/mL. 20 ng/mL. 40 ng/ml.. 200 ng/ml. and 400 ng/ml. so as to obtain standard solutions.
7. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to claim 1 or 2. wherein the sample container is a perforated plate.
8. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to claim 7. wherein the sample container is a 96-well plate.
9. The method for rapid extraction and analysis of 10 polycyclic aromatic hydrocarbons in water according to any one of claims 1-8. wherein the parallel solid-phase membrane sheet sample pretreatment microplate system device involved in the method 1s composed of a membrane sheet system (1). the 96-well plate (2) and an oscillating device (3). and specific operations are performed according to the following steps: a. sample treatment: adding a water sample in à 96-well plate (2). placing the 96-well plate (2) in an oscillating device (3) to be oscillated by the oscillating device (3). and meanwhile adsorbing the water sample with the membrane sheet system (1) for 50 min: taking a new 96-well plate (2). adding a solution of acetonitrile and water In a Volume ratio of 80:20 in cach well. oscillating and desorbing for 50 min, and then putting the 96-well plate (2) in an automatic sample
BL-5187 injector, injecting the sample into an ultra-high performance liquid chromatograph-mass LU102485 spectrograph for analysis and detection; b, conditions of ultra-high performance liquid chromatography: chromatographic column: Hypersil GOLD, C18 100 x 2.1 mm, 1.9 pm; mobile phase: A-water, and B-acetonitrile; elution gradient: 0-2 min, A 60%; 2-3 min, A 60%-20%; 3.0-8.0 min, A 20%; 8.0-8.1 min, A 20%-60%:
8.1-10.0 min. A 60%. flow rate: 0.35 mL/min; column temperature: 30°C; injection volume: 5 pL; c. conditions of mass spectrometry: ion source current: +4.0 v; ion source temperature: 400 C : sheath gas: 35 arb; auxiliary gas: 5 arb: ion transfer capillary tube temperature: 350°C; ion source type is an atmospheric pressure chemical APCI ion source; d. preparation of control solution: precisely fetching 100 ul. of control. dissolving the control with acetonitrile to a constant volume of 1 mL as a control stock solution; e. plotting of standard curves: precisely fetching the control stock solution, respectively diluting the control stock solution into 2 ng/mL, 4 ng/mL, 20 ng/ml., 40 ng/mL, 200 ng/mL and 400 ng/mL with a diluent namely a solution having a volume ratio of water to acetonitrile being 20:80 to obtain standard solutions; performing ultra-high performance liquid chromatography- mass spectrometry according to chromatographic conditions: and performing regression analysis by concentration versus peak area, so as to obtain standard component curves. and calculating regression equations: and f. determination of contents: precisely sucking a sample to-be-detected solution, performing ultra-high performance liquid chromatography-mass spectrometry according to chromatographic conditions and introducing peak areas into the standard curves to calculate contents, wherein detection results are as follows: naphthalene 6.0-207 ng; acenaphthene 2.4~30.7 ng; acenaphthylene 1.7-48.0 ng; fluorene 5.6~60.5 ng; phenanthrene 11.1~64.2 ne: anthracene
1.06-66.8 ng: fluoranthene 5.9--52.5 ng: pyrene 3.7-70.4 ng; benzopyrene b fluoranthene 1.716 ng: benzo a pyrene 18-118 ng.
11
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