CN104133022A - Method for extracting, enriching and quantifying trace ofloxacin on suspended particulate matters in water - Google Patents
Method for extracting, enriching and quantifying trace ofloxacin on suspended particulate matters in water Download PDFInfo
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- CN104133022A CN104133022A CN201410416658.0A CN201410416658A CN104133022A CN 104133022 A CN104133022 A CN 104133022A CN 201410416658 A CN201410416658 A CN 201410416658A CN 104133022 A CN104133022 A CN 104133022A
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 22
- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 title abstract description 29
- 229960001699 ofloxacin Drugs 0.000 title abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 239000012528 membrane Substances 0.000 claims abstract description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001914 filtration Methods 0.000 claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 10
- 238000001819 mass spectrum Methods 0.000 claims abstract description 8
- 238000007664 blowing Methods 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 239000012634 fragment Substances 0.000 claims abstract description 5
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 239000000126 substance Substances 0.000 claims description 23
- UIOFUWFRIANQPC-JKIFEVAISA-N Floxacillin Chemical compound N([C@@H]1C(N2[C@H](C(C)(C)S[C@@H]21)C(O)=O)=O)C(=O)C1=C(C)ON=C1C1=C(F)C=CC=C1Cl UIOFUWFRIANQPC-JKIFEVAISA-N 0.000 claims description 18
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 229960004273 floxacillin Drugs 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 238000004445 quantitative analysis Methods 0.000 claims description 15
- 238000000605 extraction Methods 0.000 claims description 10
- 239000007791 liquid phase Substances 0.000 claims description 9
- 238000005374 membrane filtration Methods 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 7
- 150000001875 compounds Chemical class 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 6
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000004704 ultra performance liquid chromatography Methods 0.000 claims description 6
- 238000004949 mass spectrometry Methods 0.000 claims description 5
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 235000019253 formic acid Nutrition 0.000 claims description 3
- 238000005286 illumination Methods 0.000 claims description 3
- 229960002422 lomefloxacin Drugs 0.000 claims description 3
- ZEKZLJVOYLTDKK-UHFFFAOYSA-N lomefloxacin Chemical compound FC1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNC(C)C1 ZEKZLJVOYLTDKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000003960 organic solvent Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 230000008719 thickening Effects 0.000 claims description 3
- 238000002137 ultrasound extraction Methods 0.000 claims description 3
- XBHBWNFJWIASRO-UHFFFAOYSA-N 6-fluoro-1-(4-fluorophenyl)-4-oxo-7-(1-piperazinyl)-3-quinolinecarboxylic acid Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1=CC=C(F)C=C1 XBHBWNFJWIASRO-UHFFFAOYSA-N 0.000 claims description 2
- 229950007734 sarafloxacin Drugs 0.000 claims description 2
- 239000003643 water by type Substances 0.000 claims description 2
- 238000004128 high performance liquid chromatography Methods 0.000 abstract description 2
- 239000003242 anti bacterial agent Substances 0.000 abstract 1
- 229940088710 antibiotic agent Drugs 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 239000002274 desiccant Substances 0.000 abstract 1
- 229910001873 dinitrogen Inorganic materials 0.000 abstract 1
- 238000010813 internal standard method Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 238000007789 sealing Methods 0.000 abstract 1
- 239000002245 particle Substances 0.000 description 7
- 150000002500 ions Chemical class 0.000 description 6
- 241000894006 Bacteria Species 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 3
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 3
- 239000003651 drinking water Substances 0.000 description 2
- 229940124307 fluoroquinolone Drugs 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000004451 qualitative analysis Methods 0.000 description 2
- 241000193830 Bacillus <bacterium> Species 0.000 description 1
- RJQXTJLFIWVMTO-TYNCELHUSA-N Methicillin Chemical compound COC1=CC=CC(OC)=C1C(=O)N[C@@H]1C(=O)N2[C@@H](C(O)=O)C(C)(C)S[C@@H]21 RJQXTJLFIWVMTO-TYNCELHUSA-N 0.000 description 1
- 108060004795 Methyltransferase Proteins 0.000 description 1
- 241000202934 Mycoplasma pneumoniae Species 0.000 description 1
- 241000588653 Neisseria Species 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000009513 drug distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 210000003608 fece Anatomy 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 229960003085 meticillin Drugs 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- LISFMEBWQUVKPJ-UHFFFAOYSA-N quinolin-2-ol Chemical compound C1=CC=C2NC(=O)C=CC2=C1 LISFMEBWQUVKPJ-UHFFFAOYSA-N 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention discloses a method for extracting, enriching and quantifying trace ofloxacin on suspended particulate matters in water. The method comprises the following steps: filtering a target water sample by using a micro-pore fiber membrane; collecting the fiber membrane subjected to filtration; airing the fiber membrane and cutting the fiber membrane into fragments; putting the fragments into a triangular flask; adding an extracting agent and sealing the triangular flask; oscillating and extracting by ultrasonic waves; filtering extracting liquid by using an organic fiber membrane; meanwhile, transferring the filtered extracting liquid into a K-D concentration bottle; adding a dehydration drying agent into an extracted filtering liquid; after absorbing water, putting the K-D concentration bottle into a rotary evaporator and concentrating; blowing the concentrated liquid by use of nitrogen gas until the volume is smaller than 1mL; making up the volume of the concentrated extracted filtering liquid to be 1mL and transferring the concentrated extracted filtering liquid to an Agilent special bottle; detecting the liquid by adopting an internal standard method through a high performance liquid chromatography cascaded three-grade gas chromatograph-mass spectrometer; and analyzing a chromatograph-mass spectrum analysis pattern to finish detection. According to the method, the content of the ofloxacin adsorbed on the suspended particulate matters in a water environment can be supplemented and the blank of the detection of antibiotics can be filled.
Description
Technical field
The invention belongs to environmental monitoring technology field, relate to the detection method of Ofloxacin in a kind of water environment, be specifically related in a kind of water the quantivative approach of Ofloxacin extracting and enriching on particle.
Background technology
Ofloxacin is a kind of artificial synthetic, antibacterial fluoroquinolones of high-efficiency broad spectrum, grampostive bacteria (including methicillin-resistant staphylococcus aureus) and gram-negative bacteria (comprising Pseudomonas aeruginosa) are all had and pretend use, mycoplasma pneumoniae, Neisseria, anaerobion and tubercle bacillus are also had to certain activity.It is by acting on the A subunit of DNA of bacteria helicase, suppresses the synthetic of DNA and copies and cause bacterium death.
Ofloxacin was synthesized in nineteen eighty-two, and oral easy absorption is fast and completely, blood concentration is high and lasting, and drug distribution is wide, was comparatively outstanding kind in generally acknowledged quinolone medicine.Because frequency of utilization is high, bacterium is also day by day increased the resistance phenomenon of its generation, and in human body the complete residual Ofloxacin of metabolism not, flow in water environment by excreta.In recent years, in water environment, the report of trace oxygen Flucloxacillin was a lot of both at home and abroad, and concentration is the magnitude to μ g/L by ng/L, and the Ofloxacin in these water environments, finally enters into potable water system by water intaking, the effectively Technology Need exploitation of Ofloxacin in degradation water.Therefore,, in order to ensure drinking water safety, accurately detect in water environment, the method for trace oxygen Flucloxacillin is indispensable prerequisite in water treatment system.At present, both at home and abroad at extracting and enriching and the quantitative technical also development that detects underwater trace Ofloxacin, common report has the method for the collaborative using high performance liquid chromatography tandem mass spectrum of Solid-Phase Extraction, before carrying out Solid-Phase Extraction, all water samples need to be through the membrane filtration of 0.45 μ m, the Ofloxacin of solubilised state, after Solid-Phase Extraction, after enrichment, detects.These methods be confined to solubilised state Ofloxacin quantitatively on.Studies have reported that, Ofloxacin belongs to carboxylic acid material, be easy to be adsorbed on particle surface, therefore, the necessary extraction of the Ofloxacin on particle surface is got off, carry out quantitatively, like this, pollution situation that can omnibearing grasp water oxygen Flucloxacillin, is to resolve the Transport of Ofloxacin in water environment, attenuation law in water treatment system, has important supporting role.
Summary of the invention
The object of this invention is to provide in a kind of water trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance.
The object of the invention is by below data-selected scheme being realized:
(1) get target water sample 2000-4000ml, use microporous fibre membrane filtration, collect filter membrane and the surperficial suspended particulate substance of holding back after filtering, after filter membrane is dried, be cut into fragment and be placed in triangular flask, measure appropriate extractant with graduated cylinder and pour in triangular flask; Be placed in shaken cultivation case with sealed membrane good seal, Temperature Setting is 4-10 DEG C, closes illumination and makes its dark, speed setting is 100-200 time/min, after vibration 8-12h, triangular flask is taken out, carry out ultrasonic extraction, extraction time 20-35min, is extracted liquid.
(2) extract obtaining by organic membrane filtration step 1 is transferred to the extract after filtering in the concentrated bottle of K-D simultaneously.
(3) add and dehydrate agent to the extraction filtered fluid in the concentrated bottle of step 2 K-D, after wipe dry, concentrated K-D bottle is put into rotary evaporator and concentrate, thickening temperature 30-45 DEG C, the time is 10-20min, concentrated after volume be that 1-2ml is advisable.
(4) liquid after step 3 is concentrated, with nitrogen blowing to volume be, below 1ml, to stop nitrogen blowing.
(5) concentrate extraction filtered fluid step 4 being obtained is settled to 1mL, and the liquid rotating after constant volume is moved on in Agilent special-purpose bottle.
(6) in the liquid to be measured obtaining in step 5, add the internal standard compound of 0.5ml, then in three grades of mass spectrometry instruments of ultrahigh pressure liquid phase chromatogram series connection, detect, detected parameters is as follows:
Liquid-phase condition: a) mobile phase composition: A.0.2vol.% formic acid, B. methyl alcohol; B) sample size: 10 μ L; C) flow velocity: 0.2 mL/min; D) column temperature: 30 DEG C; E) working time: 8min; F) chromatographic column: Acquity UPLC BEH; G) gradient: as shown in table 1.
Mass spectrum condition: a) desolventizing temperature degree: 350 DEG C; B) source temperature: 150 DEG C; C) capillary voltage: 3000V; D) desolventizing gas velocity: 650L/h; E) cone gas velocity: 50L/h.Quantitative and qualitative analysis ion is set in table 2.
(7) chromatograph mass spectrum analysis figure is analyzed, complete detection.
In said method, the aperture of the described microporous fiber membranes of step (1) is 0.45 μ m.
In said method, the described quality of suspended particulate substance and the volume ratio of extractant of step (1) is 1g:15-20ml.
In said method, the described extractant of step (1) is methyl alcohol.
In said method, the described oscillator of step (1) is the HZQ-F160 type shaken cultivation case of HDL company, and rotating speed is 100-200 time/min; Ultrasonic extracting machine is KQ-100DE type ultrasonic extracting machine, and ultrasonic frequency is 23-40kHz.
In said method, the aperture of the described organic filter membrane of step (2) is 0.22 μ m.
In said method, the described agent that dehydrates of step (3) is anhydrous sodium sulfate.
In said method, the described constant volume organic solvent of step (5) is methyl alcohol.
In said method, the described internal standard compound of step (6) is selected according to actual residue in water situation, and this method adopts sarafloxacin or Lomefloxacin, and structure and Ofloxacin are similar, at the NF fluoroquinolones material of target water body.Internal standard compound is not only confined to these two kinds, as long as allied substances, and its structural similarity, and do not detect and all can in detected water sample.
In said method, the described three grades of mass spectrometry instruments of ultrahigh pressure liquid phase chromatogram series connection of step (6) are Waters Xevo TQ MS Acquity UPLC System, the ultrahigh pressure liquid phase chromatographic column (Acquity UPLC BEH) that instrument carries.
Table 1 eluent gradient elution program
Qualitative and the quota ion of table 2 Ofloxacin
Note: MRM
1for quota ion, MRM
2for qualitative ion.
Tool of the present invention has the following advantages:
1, adopt method provided by the invention, can detect the content of the Ofloxacin adsorbing on suspended particulate substance in water environment, reflect more really the content of water oxygen Flucloxacillin, thus the pollution situation of omnibearing grasp water oxygen Flucloxacillin.
2, this method is to resolve the Transport of Ofloxacin in water environment, and the attenuation law in water treatment system, has important supporting role.
3, this method has been supplemented the content of the Ofloxacin adsorbing on suspended particulate substance in water environment, has supplemented the blank that microbiotic detects.
Brief description of the drawings
Fig. 1 is particle extracting and enriching overhaul flow chart.
Embodiment
Below technical scheme of the present invention is further described, but does not limit to so, every technical solution of the present invention is modified or is equal to replacement, and do not depart from the spirit and scope of technical solution of the present invention, all should be encompassed in protection scope of the present invention.
As shown in Figure 1, trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water provided by the invention, its concrete implementation step is as follows:
(1) get target water sample 2000ml, with 0.45 μ m microporous fibre membrane filtration, collect the filter membrane after filtering, after filter membrane is dried, be cut into fragment and be placed in triangular flask, measure appropriate methyl alcohol with graduated cylinder and pour in triangular flask, the quality of described suspended particulate substance and the volume ratio of methyl alcohol are 1g:20ml; Be placed in shaken cultivation case with sealed membrane good seal, Temperature Setting is 4 DEG C, closes illumination and makes its dark, and speed setting is 100 times/min, after vibration 8h, triangular flask is taken out, and carries out ultrasonic extraction, and extraction time 35min, is extracted liquid.
(2) extract obtaining by the organic membrane filtration step 1 of 0.22 μ m is transferred to the extract after filtering in the concentrated bottle of K-D simultaneously.
(3) add anhydrous sodium sulfate to concentrate the extraction filtered fluid in bottle to step 2 K-D, after wipe dry, concentrated K-D bottle is put into rotary evaporator and concentrate, 30 DEG C of thickening temperatures, the time is 20min, concentrated rear volume is 1ml.
(4) liquid after step 3 is concentrated, with nitrogen blowing to volume be, below 1ml, to stop nitrogen blowing.
(5) the concentrate extraction filtered fluid with methyl alcohol, step 4 being obtained is settled to 1mL, and the liquid rotating after constant volume is moved on in Agilent special-purpose bottle.
(6) in the liquid to be measured obtaining in step 5, add 0.5ml internal standard compound Lomefloxacin (concentration 10 μ g/L), then in three grades of mass spectrometry instruments of ultrahigh pressure liquid phase chromatogram series connection, detect, detected parameters is as follows:
Liquid-phase condition: a) mobile phase composition: A.0.2% formic acid, B. methyl alcohol; B) sample size: 10 μ L; C) flow velocity: 0.2 mL/min; D) column temperature: 30 DEG C; E) working time: 8min; F) chromatographic column: Acquity UPLC BEH; G) gradient: as shown in table 1.
Mass spectrum condition: a) desolventizing temperature degree: 350 DEG C; B) source temperature: 150 DEG C; C) capillary voltage: 3000V; D) desolventizing gas velocity: 650L/h; E) cone gas velocity: 50L/h.Quantitative and qualitative analysis ion is set in table 3.
(7) chromatograph mass spectrum analysis figure is analyzed, complete detection.
Table 4 is analysis results of 3 sub-samplings of the inventive method to the Ofloxacin on solubilised state and suspended particulate substance in the Yuan Shui of Song Hua River.Visible, on particle, adhere to a certain amount of Ofloxacin, the highest ratio is more than 15%.Illustrate, the detection of Ofloxacin in water environment, can not ignore the part of adsorbing on suspended particulate substance.
Qualitative and the quota ion of table 3 Ofloxacin
Table 4 testing result
| Project | The content (ng/L) of solubilised state Ofloxacin in 0.45 μ m membrane filtration water | The content (ng/L) of suspended particle Ofloxacin on 0.45 μ m membrane filtration film | On particle, Ofloxacin accounts for the ratio % of solubilised state Ofloxacin |
| Water sample 1 | 55.09±2.80 | 4.20±1.32 | 7.6 |
| Water sample 2 | 35.00±3.74 | 3.74±1.16 | 10.6 |
| Water sample 3 | 29.15±1.37 | 4.60±0.04 | 15.8 |
Claims (10)
1. trace oxygen Flucloxacillin extracting and enriching and a quantitative method on suspended particulate substance in water, is characterized in that described method step is as follows:
(1) get target water sample 2000-4000ml, use microporous fibre membrane filtration, collect filter membrane and the surperficial suspended particulate substance of holding back after filtering, after filter membrane is dried, be cut into fragment and be placed in triangular flask, measure appropriate extractant with graduated cylinder and pour in triangular flask, controlling the quality of suspended particulate substance and the volume ratio of extractant is 1g:15-20ml; Be placed in shaken cultivation case with sealed membrane good seal, Temperature Setting is 4-10 DEG C, closes illumination and makes its dark, speed setting is 100-200 time/min, after vibration 8-12h, triangular flask is taken out, carry out ultrasonic extraction, extraction time 20-35min, is extracted liquid;
(2) extract obtaining by organic membrane filtration step 1 is transferred to the extract after filtering in the concentrated bottle of K-D simultaneously;
(3) add and dehydrate agent to the extraction filtered fluid in the concentrated bottle of step 2 K-D, after wipe dry, concentrated K-D bottle is put into rotary evaporator and concentrate, thickening temperature 30-45 DEG C, the time is 10-20min;
(4) liquid after step 3 is concentrated, with nitrogen blowing to volume be, below 1ml, to stop nitrogen blowing;
(5) add organic solvent, the concentrate extraction filtered fluid that step 4 is obtained is settled to 1mL, and the liquid rotating after constant volume is moved on in Agilent special-purpose bottle;
(6) in the liquid to be measured obtaining in step 5, add the internal standard compound of 0.5ml, then in three grades of mass spectrometry instruments of ultrahigh pressure liquid phase chromatogram series connection, detect;
(7) chromatograph mass spectrum analysis figure is analyzed, complete detection.
2. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the aperture of the described microporous fiber membranes of step (1) is 0.45 μ m.
3. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the described extractant of step (1) is methyl alcohol.
4. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the described ultrasonic frequency of step (1) is 23-40kHz.
5. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the aperture of the described organic filter membrane of step (2) is 0.22 μ m.
6. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the described agent that dehydrates of step (3) is anhydrous sodium sulfate.
7. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the liquid volume after described concentrated of step (3) is 1-2ml.
8. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the described constant volume organic solvent of step (5) is methyl alcohol.
9. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, is characterized in that the described internal standard compound of step (6) is sarafloxacin or Lomefloxacin.
10. trace oxygen Flucloxacillin extracting and enriching and quantitative method on suspended particulate substance in water according to claim 1, it is characterized in that the described three grades of mass spectrometry instruments of ultrahigh pressure liquid phase chromatogram string series connection of step (6) are Waters Xevo TQ MS Acquity UPLC System, detected parameters is as follows:
Liquid-phase condition: a) mobile phase composition: A.0.2vol.% formic acid, B. methyl alcohol; B) sample size: 10 μ L; C) flow velocity: 0.2 mL/min; D) column temperature: 30 DEG C; E) working time: 8min; F) chromatographic column: Acquity UPLC BEH; G) gradient: 0min:V (A) %-80, V (B) %-20,5min:V (A) %-30, V (B) %-70,5.1min:V (A) %-0, V (B) %-100,6.5min:V (A) %-0, V (B) %-100,6.6min:V (A) %-80, V (B) %-20,8min:V (A) %-80, V (B) %-20;
Mass spectrum condition: a) desolventizing temperature degree: 350 DEG C; B) source temperature: 150 DEG C; C) capillary voltage: 3000V; D) desolventizing gas velocity: 650L/h; E) cone gas velocity: 50L/h.
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Cited By (2)
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| CN110333301A (en) * | 2019-06-24 | 2019-10-15 | 广东省测试分析研究所（中国广州分析测试中心） | Method that is a kind of while measuring 9 kinds of sulfa antibiotics on suspended particulate substance in water |
| CN114428137A (en) * | 2022-01-28 | 2022-05-03 | 中国科学院东北地理与农业生态研究所 | Trace detection method for suspended particulate matters in water body |
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|---|---|---|---|---|
| CN110333301A (en) * | 2019-06-24 | 2019-10-15 | 广东省测试分析研究所（中国广州分析测试中心） | Method that is a kind of while measuring 9 kinds of sulfa antibiotics on suspended particulate substance in water |
| CN114428137A (en) * | 2022-01-28 | 2022-05-03 | 中国科学院东北地理与农业生态研究所 | Trace detection method for suspended particulate matters in water body |
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