CN102128897A - Ultrasound-assisted emulsification-microextraction method for pretreatment of artificially synthesized musk in water body - Google Patents
Ultrasound-assisted emulsification-microextraction method for pretreatment of artificially synthesized musk in water body Download PDFInfo
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- CN102128897A CN102128897A CN 201010577888 CN201010577888A CN102128897A CN 102128897 A CN102128897 A CN 102128897A CN 201010577888 CN201010577888 CN 201010577888 CN 201010577888 A CN201010577888 A CN 201010577888A CN 102128897 A CN102128897 A CN 102128897A
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Abstract
The invention provides an ultrasound-assisted emulsification-microextraction (USAEME) method for pretreatment of artificially synthesized musk in a water body, belongs to the technical field of analytical chemistry, and particularly relates to the technical field of detection of water environment pollutants. The method using the USAEME in the pretreatment of the artificially synthesized musk comprises the following treatment steps of: adding a sample, adding an extracting agent, performing ultrasonic oscillation to form an emulsion system, performing centrifugal separation, absorbing an organic phase and directly performing gas chromatography-mass spectrometry. The method has the advantages of high enrichment capacity, simple operation, low organic solvent consumption and short extraction time, integrates sampling, extraction and concentration, avoids the possible problem of cross contamination, is a simple, quick, low-cost, efficient and environmentally-friendly sample pretreatment technology, and can quickly analyze artificially synthesized musk content of the water.
Description
Technical field
A kind of ultrasonic auxiliary emulsion liquid microextraction method that is used for the pre-treatment of water body synthetic Moschus belongs to the analytical chemistry field, more specifically relates to the detection technique field of water environment pollution thing.The present invention designs with ultrasonic auxiliary emulsification method, with carrying out quantitative test behind eight kinds of common synthetic Moschus in the chlorobenzene extraction water body.
Background technology
The synthetic Moschus is with its graceful aromatic odor, and good fixation ability and cheap price have replaced natural musk, are widely used in the products such as cosmetics, articles for washing, skin care item, perfume.The synthetic Moschus has become a kind of persistent pollutant in the environment, is classified as an important component part of medicine and personal-care supplies (PPCPs).A large amount of uses along with various commodity, the synthetic Moschus will enter in the environment along with sanitary sewage, all detect the synthetic Moschus in existing superficial water, sewage, activated sludge, sediment, atmosphere, the aquatic animal, even in people's adipose tissue, blood, breast milk, also detected the synthetic Moschus.
The synthetic Moschus pollutes the use mainly due to various daily chemical products, and along with the discharging of sanitary sewage, what at first be subjected to the pollution of synthetic Moschus is water environment, again via each corner in the water environment arrival environment.The extraction and analytical method of synthetic Moschus is mainly in the water environment: liquid-liquid extraction (LLE), Solid-Phase Extraction (SPE) and solid-phase microextraction (SPME).But LLE need consume a large amount of poisonous organic solvents, complicated operation, and time-consuming, be difficult to realize the processing of robotization and a large amount of samples.SPE uses more convenient than LLE, has very strong selectivity, but price is relatively expensive.SPME is a kind of solvent-free abstraction technique, but costs an arm and a leg, extracting head relatively fragility and serviceable life shorter.In recent years, ultrasonic auxiliary emulsification liquid-liquid micro-extraction (USAEME) successfully has been used for the extraction of the multiple trace organic substance of aqueous solution as a kind of new abstraction technique, as phthalic ester, and lindane and PBDE etc.USAEME makes the organic extractant generation uniformly emulsify of trace in the aqueous solution based on ultrasound wave, and reaches the mass transfer balance rapidly, reaches the purpose of extraction organic contaminant; By centrifugal organic phase and the aqueous phase separation of making, organic phase can be directly used in gas phase or makings analysis.The organic extractant that USAEME adopts is considerably less, makes this method have higher extracting and enriching multiple, thereby obtains lower detectability and very high sensitivity.Therefore, USAEME is considered to a kind of efficient, easy, quick, cheap and free of contamination abstraction technique.
With ultrasonic auxiliary emulsion liquid microextraction method the method for the synthetic Moschus pre-treatment in the water body is not seen bibliographical information as yet.
Summary of the invention
The object of the present invention is to provide the method for synthetic Moschus pre-treatment in a kind of water body, adopt ultrasonic auxiliary emulsification method, with 8 kinds of synthetic Moschus (opening Xu Meilong (DPMI), celestolide (ADBI), phantolid (AHMI), Te Lasi (ATII), Jiale muskiness (HHCB), tonalid (AHTN), musk xylene (MX) and muskone (MK)) the back quantitative test in the chlorobenzene extraction water body of trace.This method accumulation ability height, simple to operate, consumption of organic solvent is few and the extraction time short, and cost is low.
Technical scheme of the present invention: a kind of ultrasonic auxiliary emulsion liquid microextraction method that is used for the pre-treatment of water body synthetic Moschus, measure a certain amount of water sample and with a small amount of chlorobenzene as extraction solvent, adopt ultrasonic auxiliary emulsifying manner, make the synthetic Moschus be extracted in the organic phase rapidly, by centrifugal organic phase and the aqueous phase separation of making, organic phase can be directly used in gas chromatography-mass spectrometry analysis.Step is:
A. membrane filtration preliminary clearning: get water sample to be detected, collect filtrate behind the filter membrane through 0.45 μ m;
B. get sample liquid after the steps A of 10.0mL in 15mL taper centrifuge tube with cover, mark in adding: after 10 μ L concentration are the hexane solution of 100ng/mL hexamethylbenzene (HMB), add 50-100 μ L extraction solvent chlorobenzene;
C. the taper centrifuge tube is placed the ultrasonic 10min of ultrasonoscope, keep simultaneously that water temperature is 30 ℃ in the Ultrasound Instrument;
D. with the taper centrifuge tube with the centrifugal 10-15min of 4000 r/min;
E. the chlorobenzene solution with micro-liquid phase sample introduction needle absorption centrifuge tube bottom directly advances gas chromatography-mass spectrometry analysis.
The described taper centrifuge tube of step B is the taper centrifuge tube with cover that the bottom has good visibility.
Gas chromatography-mass spectrometry analysis (GC-MS) condition:
GC conditions: chromatographic column: DB-WAX capillary chromatographic column, 30 m * 0.25 mm * 0.25 μ m; Carrier gas: high-purity He(99.995%), flow velocity: 1.0mLmin
-1No split sampling, sample size 1 μ L; 280 ℃ of injector temperatures; 130 ℃ of post beginning temperature keep 0.5min, with 12 ℃ of min
-1Speed rise to 230 ℃, keep 12min.
Mass spectrum condition: EI source; 200 ℃ of ion source temperatures; Interface temperature: 250 ℃; Select the ion monitoring pattern, target compound is qualitative with retention time and characteristic ion.Concentration according to calculated by peak area synthetic Moschus.
The stratographic analysis retention time of interior mark and 8 kinds of synthetic Moschus and monitoring ion see the following form:
| Compound | Retention time (min) | Qualitative ion | Quota ion |
| HMB | 6.92 | 162 | 147 |
| DPMI | 7.43 | 206 | 191 |
| ADBI | 9.70 | 244 | 229 |
| AHMI | 10.68 | 244 | 229 |
| HHCB | 11.00 | 258 | 243 |
| ATII | 11.37 | 258 | 215 |
| AHTN | 11.70 | 258 | 215 |
| MX | 13.22 | 294 | 279 |
| MK | 18.43 | 297 | 282 |
The ultrasonic auxiliary emulsification liquid-liquid micro-extraction that the present invention sets up-gas chromatography combined with mass spectrometry is measured 8 kinds of synthetic Moschus in the aqueous solution.Detecting of this method is limited to 0.0030-0.0050 ng/mL; In the scope of concentration 1-80 ng/mL, peak area and sample concentration are the good linear relation.
Beneficial effect of the present invention:
The inventive method accumulation ability height, simple to operate, consumption of organic solvent is few and the extraction time short, the centralized procurement sample, extract and when concentrating in one, avoided may problem, the problem includes: the problem of cross pollution, be a kind of simple, fast, cost is low, efficient and eco-friendly sample pre-treatments technology, the synthetic Moschus content in can express-analysis water.
Description of drawings
Fig. 1 is in conjunction with the process flow diagram of USAEME device of the present invention.Wherein, to locate be 100 μ L liquid phase micro syringes (2), (5).
Fig. 2 synthetic Moschus standard specimen (20 ng/mL) chromatogram.
Fig. 3 actual water sample product chromatogram.
Embodiment
Embodiment 1:
1, the sample after the collection is crossed 0.45 μ m filter membrane.
2, the above-mentioned filtrate of getting 10.0mL is in 15mL taper centrifuge tube with cover, and mark in adding: 10 μ L concentration are the hexane solution of 100ng/mL hexamethylbenzene (HMB), add 50 μ L extraction solvent chlorobenzenes.
3, the taper centrifuge tube is placed the ultrasonic 10min of ultrasonoscope, keep simultaneously that water temperature is 30 ℃ in the Ultrasound Instrument.
4, with the taper centrifuge tube with the centrifugal 10min of 4000r/min.
5, the chlorobenzene with micro-liquid phase sample introduction needle absorption centrifuge tube bottom directly advances gas chromatography-mass spectrometry analysis.
6, the content detection of 8 kinds of synthetic Moschus adopts the GC-MS method.Chromatographic column: DB-WAX capillary chromatographic column, 30 m * 0.25 mm * 0.25 μ m; Carrier gas: high-purity He(99.995%), flow velocity: 1.0mLmin
-1No split sampling, sample size 1 μ L; 280 ℃ of injector temperatures; 130 ℃ of post beginning temperature keep 0.5min, with 12 ℃ of min
-1Speed rise to 230 ℃, keep 12min.
Mass spectrum condition: EI source; 200 ℃ of ion source temperatures; Interface temperature: 250 ℃; Select the ion monitoring pattern, target compound is qualitative with retention time and characteristic ion, according to the concentration of calculated by peak area synthetic Moschus.
Embodiment 2:
1, the sample after the collection is crossed 0.45 μ m filter membrane.
2, the above-mentioned filtrate of getting 10.0mL is in 15mL taper centrifuge tube with cover, and mark in adding: 10 μ L concentration are the hexane solution of 100ng/mL hexamethylbenzene (HMB), add 100 μ L extraction solvent chlorobenzenes.
3, the taper centrifuge tube is placed the ultrasonic 10min of ultrasonoscope, keep simultaneously that water temperature is 30 ℃ in the Ultrasound Instrument.
4, with the taper centrifuge tube with the centrifugal 15min of 4000r/min.
5, the chlorobenzene with micro-liquid phase sample introduction needle absorption centrifuge tube bottom directly advances gas chromatography-mass spectrometry analysis.
Adopt GC-MS method testing conditions with embodiment 1.
The foregoing description is only for the usefulness of explanation invention, rather than limitation of the invention anyly all belongs to protection scope of the present invention to the scheme after the simple change of the present invention.
Claims (3)
1. ultrasonic auxiliary emulsion liquid microextraction method that is used for the pre-treatment of water body synthetic Moschus, it is characterized in that: measure a certain amount of water sample with a small amount of chlorobenzene as extraction solvent, adopt ultrasonic auxiliary emulsifying manner, make the synthetic Moschus be extracted in the organic phase rapidly, by centrifugal organic phase and the aqueous phase separation of making, organic phase is directly used in gas chromatography-mass spectrometry analysis; This method may further comprise the steps successively:
A. membrane filtration preliminary clearning: get water sample to be detected, collect filtrate behind the filter membrane through 0.45 μ m;
B. the sample liquid of getting after the steps A of 10.0mL places 15mL taper centrifuge tube with cover, and mark in adding: 10 μ L concentration are the hexane solution of 100ng/mL hexamethylbenzene, add 50-100 μ L extraction solvent chlorobenzene;
C. the taper centrifuge tube is placed the ultrasonic 10min of ultrasonoscope, keep simultaneously that water temperature is 30 ℃ in the Ultrasound Instrument;
D. with the taper centrifuge tube with the centrifugal 10-15min of 4000r/min;
E. the chlorobenzene solution with micro-liquid phase sample introduction needle absorption centrifuge tube bottom directly advances gas chromatography-mass spectrometry analysis.
2. the ultrasonic auxiliary emulsion liquid microextraction method that is used for the pre-treatment of water body synthetic Moschus according to claim 1 is characterized in that: the described taper centrifuge tube of step B is the taper centrifuge tube with cover that the bottom has good visibility.
3. the ultrasonic auxiliary emulsion liquid microextraction method that is used for the pre-treatment of water body synthetic Moschus according to claim 1, it is characterized in that: the gas chromatography-mass spectrometry analysis condition is:
GC conditions: chromatographic column: DB-WAX capillary chromatographic column, 30 m * 0.25 mm * 0.25 μ m; Carrier gas: high-purity He of 99.995%, flow velocity: 1.0mLmin
-1No split sampling, sample size 1 μ L; 280 ℃ of injector temperatures; 130 ℃ of post beginning temperature keep 0.5min, with 12 ℃ of min
-1Speed rise to 230 ℃, keep 12min;
Mass spectrum condition: EI source; 200 ℃ of ion source temperatures; Interface temperature: 250 ℃; Select the ion monitoring pattern, target compound is qualitative with retention time and characteristic ion, according to the concentration of calculated by peak area synthetic Moschus.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914597A (en) * | 2011-08-02 | 2013-02-06 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| CN104568562A (en) * | 2014-12-31 | 2015-04-29 | 中国地质大学（武汉） | Water sample and pretreatment method of nitrosoamine compound in suspended matter of water sample |
| CN108760924A (en) * | 2018-05-31 | 2018-11-06 | 河南中烟工业有限责任公司 | A kind of extraction detection method of filter stick perfume (or spice) line and quick-fried pearl characteristic component |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334391A (en) * | 2008-07-16 | 2008-12-31 | 上海大学 | Method for determining synthetic musk concentration of breast milk |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101334391A (en) * | 2008-07-16 | 2008-12-31 | 上海大学 | Method for determining synthetic musk concentration of breast milk |
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Chromatography A》 20081231 Jorge Regueiro et al. Ultrasound-assisted emulsification- microextraction of emergent contaminants and pesticides in environmental waters 27-38 1-3 第1190卷, * |
| 《环境化学》 20100131 梁高锋等 气相色谱-质谱联用测定母乳中合成麝香 第29卷, 第1期 * |
| 《环境化学》 20100531 胡正君等 气相色谱-质谱法测定人体血液样品中合成麝香 530-535 第29卷, 第3期 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102914597A (en) * | 2011-08-02 | 2013-02-06 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| CN102914597B (en) * | 2011-08-02 | 2014-10-15 | 漳州片仔癀药业股份有限公司 | Quality testing method for fingerprint of herbal medicine musk |
| CN104568562A (en) * | 2014-12-31 | 2015-04-29 | 中国地质大学（武汉） | Water sample and pretreatment method of nitrosoamine compound in suspended matter of water sample |
| CN108760924A (en) * | 2018-05-31 | 2018-11-06 | 河南中烟工业有限责任公司 | A kind of extraction detection method of filter stick perfume (or spice) line and quick-fried pearl characteristic component |
| CN108760924B (en) * | 2018-05-31 | 2021-04-20 | 河南中烟工业有限责任公司 | Method for extracting and detecting characteristic components of fragrant threads and popping beads of filter sticks |
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Application publication date: 20110720 |