CN103954703B - Without condensation and the method for melting collection extractant mensuration bisphenol-A again - Google Patents
Without condensation and the method for melting collection extractant mensuration bisphenol-A again Download PDFInfo
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- CN103954703B CN103954703B CN201410164857.7A CN201410164857A CN103954703B CN 103954703 B CN103954703 B CN 103954703B CN 201410164857 A CN201410164857 A CN 201410164857A CN 103954703 B CN103954703 B CN 103954703B
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Abstract
The invention discloses a kind of without condensation and the method for melting collection extractant mensuration bisphenol-A again, it comprises step: (1) is based on the vortex auxiliary liquid phase extraction of extractant gathering-device; (2) based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device.This method proposes a kind of scheme utilizing extractant gathering-device to collect microextraction agent first, saves the steps such as Ning Gu ﹑ thawing, can improve the separation and consentration efficiency of bisphenol-A in water, accelerate analysis speed.The inventive method Ju has Kuai Su ﹑ Ling Min ﹑ Zhun Que ﹑ advantages of environment protection.
Description
technical field:
The present invention relates to a kind of without condensation and again melt collect extractant device and for bisphenol-A method for measuring, the method of bisphenol-A in the detection water that specifically a kind of Jian Bian ﹑ Kuai Su ﹑ is sensitive, this method with vortex liquid-phase micro-extraction for Sample Pretreatment Technique Used, in conjunction with extractant gathering-device, utilize high performance liquid chromatography for detecting instrument.Just the fast fast ﹑ of ﹑ is highly sensitive for Fang Fajian.
background technology:
The whole world produces 2,700 ten thousand tons of plastics containing bisphenol-A now every year, bisphenol-A is ubiquitous, from mineral water bottle, medicine equipment to and packaging for foodstuff inside, have its figure, the report that widely used bisphenol-A causes the various environment support comprising water body to have it to detect.Numerous research data is verified, and bisphenol-A can cause endocrinopathy, is a kind of incretion interferent, can serious threat fetus and children healthy.Separately have data to show, the obesity that cancer and metabolic disturbance cause also is polluted with bisphenol-A substantial connection.
In water body, the detection of bisphenol-A has more report, comprises the instruments such as gas chromatography-mass spectrography (GC/MS), gas chromatography tandem mass spectrometry coupling (GC/MS/MS), liquid chromatograph mass spectrography (LC/MS), Liquid Chromatography-tandem Mass (LC/MS/MS) and is used to detect bisphenol-A in water.The Sample Pretreatment Technique Used that these analytical approachs adopt mostly is liquid-liquid extraction and these classic methods of Solid-Phase Extraction, and these method organic solvent consumptions are large, and the cycle is long, and analysis efficiency is low.Recently, liquid-phase micro-extraction, due to the low and higher analysis efficiency of its organic solvent consumption, obtains analytical work person and more and more favors.And in dispersive liquid-liquid microextraction, the organic solvent that the toxicity due to the little organic solvent of density ratio water is large compared with density ratio water is little, and analytical work person is healthy for protection, be more prone to use organic solvent that density ratio water is little as extractant.When the extractant using density ratio water little, the collection of extractant needs condensation and melts two steps again, and this greatly reduces the analysis efficiency of liquid-phase micro-extraction.
summary of the invention:
The present invention be directed to liquid-phase micro-extraction pre-treatment step in bisphenol-A mensuration process more, the problem that analysis efficiency is lower, provide a kind of without condensation and again melt collect extractant device and for bisphenol-A method for measuring.
Technical scheme of the present invention is as follows:
Without condensation and the method for melting collection extractant mensuration bisphenol-A again, it comprises step:
(1) based on the vortex auxiliary liquid phase extraction of extractant gathering-device;
(2) based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device.
Foregoing method, preferred scheme is, step (1) is utilize extractant gathering-device based on the vortex auxiliary liquid phase extraction of extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize turbula shaker to carry out vortex to water sample and extractant system, extractant is broken for the vortex auxiliary liquid phase extraction that fine drop accelerates rate of extraction.
Foregoing method, preferred scheme is, described extractant gathering-device is made up of glass tube (1) and glass tube (2), water sample to be determined contained by glass tube (2), and two ends internal diameter is identical, and glass tube (1) two ends internal diameter has a long way to go, butt end external diameter is slightly less than the internal diameter of glass tube (2), just cover glass tube (2) top water sample liquid level, taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle.
Foregoing method, preferred scheme is, step (2) is based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283nm, emission wavelength 323nm.
Foregoing method, preferred scheme is, liquid-phase chromatographic column C18 (250mm × 4.6mm, 5 μm) chromatographic column, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is become 7:3 in 5:5,15min, flow rate of mobile phase 1.0mLmin
-1.
The analytical approach of bisphenol-A in a kind of water provided by the invention, takes method to be (1) based on the vortex auxiliary liquid phase extraction (2) of extractant gathering-device based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device.In described step (1), extractant gathering-device is for shown in Fig. 1, and be made up of glass tube 1 and glass tube 2, glass tube 2 holds water, and two ends internal diameter is identical.Glass tube 1 two ends internal diameter has a long way to go, and butt end external diameter is slightly less than the internal diameter of glass tube 2, just can cover water sample liquid level above glass tube 2, and taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle.In described step (1), water sampling is placed in the glass tube of extractant gathering-device, using micro-isooctyl alcohol as extractant.Utilize turbula shaker to carry out vortex to water sample and extractant system, extractant is broken for fine drop and accelerates rate of extraction.In described step (1), extraction drop little for density ratio water is covered on the larger one end of glass tube 1 internal diameter, slowly decline glass tube, and extraction drop rises to the tiny one end of internal diameter, forms higher extractant liquid level.In described step (1), extractant suction means is liquid chromatography micro-sampling pin, draws the extractant collected.In described step (2), bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283nm, emission wavelength 323nm.In described step (2), liquid phase chromatogram condition is: liquid-phase chromatographic column C18 (250mm × 4.6mm, 5 μm) chromatographic column, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is become 7:3 in 5:5,15min, flow rate of mobile phase 1.0mLmin
-1.
Beneficial effect of the present invention is: the bisphenol-A in Ke Yi Kuai Su ﹑ sensitive analysis water.This method proposes a kind of scheme utilizing extractant gathering-device to collect microextraction agent first, saves the steps such as Ning Gu ﹑ thawing, utilizes high performance liquid chromatograph to detect bisphenol-A, Fang method Kuai Su ﹑ Ling Min ﹑ Zhun Que ﹑ environmental friendliness.
Accompanying drawing explanation
Fig. 1 is extractant gathering-device structural representation.
Fig. 2 is that bisphenol-A analyzes overhaul flow chart.
Fig. 3 is high-efficient liquid phase chromatogram after the former water high-efficient liquid phase chromatogram of certain river and mark-on.
Embodiment
Below by embodiment, the invention will be further described, to help better to understand content of the present invention, but the protection domain that these embodiments do not limit the present invention in any way.
Embodiment 1 is without condensation and melt the method for collecting extractant mensuration bisphenol-A again, comprises step:
(1) based on the vortex auxiliary liquid phase extraction of extractant gathering-device: utilize extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize turbula shaker to carry out vortex to water sample and extractant system, extractant is broken for the vortex auxiliary liquid phase extraction that fine drop accelerates rate of extraction; Described extractant gathering-device is made up of glass tube 1 and glass tube 2, water sample to be determined contained by glass tube 2, two ends internal diameter is identical, glass tube 1 two ends internal diameter has a long way to go, butt end external diameter is slightly less than the internal diameter of glass tube 2, just cover water sample liquid level above glass tube 2, taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle.
(2) based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283nm, emission wavelength 323nm.Liquid phase chromatogram condition is: liquid-phase chromatographic column C18 (250mm × 4.6mm, 5 μm) chromatographic column, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is become 7:3 in 5:5,15min, flow rate of mobile phase 1.0mLmin
-1.
The analytical approach of bisphenol-A in the former water of certain river of embodiment 2, take method to be (1) vortex auxiliary liquid phase extraction separation and concentration bisphenol-A based on extractant gathering-device, (2) are based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device.
(1) based on the vortex auxiliary liquid phase extraction separation and concentration bisphenol-A of extractant gathering-device: get the water that 5mL contains bisphenol-A and be placed in glass test tube, add 30 μ L isooctyl alcohol extractants, utilize turbula shaker to carry out the vortex auxiliary extraction of water, coextraction 90s.During vortex extraction, in water, bisphenol-A is extracted in isooctyl alcohol.After extraction, place 2min, isooctyl alcohol extractant drop floats on water liquid level because density ratio water is little.(described extractant gathering-device is made up of glass tube 1 and glass tube 2 to utilize extractant gathering-device as shown in Figure 1, water sample to be determined contained by glass tube 2, two ends internal diameter is identical, glass tube 1 two ends internal diameter has a long way to go, and butt end external diameter is slightly less than the internal diameter of glass tube 2, just covers water sample liquid level above glass tube 2, taper end internal diameter is very thin, micro-sampling pin syringe needle can just be inserted), glass device 1 is covered on ullage in glass device 2, and extraction drop is covered on the inside.Highly slowly being declined by glass device 1, slowly rises in extract dropping liquid face in glass device 1.Because glass device 2 two ends internal diameter has a long way to go, isooctyl alcohol is at the larger liquid level of the most advanced and sophisticated height of formation of glass device 2, and directly drawing 10 μ L isooctyl alcohol with micro-sampling pin carries out liquid chromatography-fluorescence detector analysis.Whole analytic process as shown in Figure 2.
(2) based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device: high-efficient liquid phase system, fluorescence and UV-detector is furnished with.During fluoroscopic examination, fluorescence detector excitation wavelength 283nm, bisphenol-A emission wavelength 323nm.Liquid-phase chromatographic column is C18 (250mm × 4.6mm, 5 μm) chromatographic column, and mobile phase is acetonitrile and water, gradient elution, starts acetonitrile: water is become 7:3 in 5:5,15min, flow rate of mobile phase 1.0mLmin
-1.
Table 1 is the correlation data of this method and other method.
Table 1 this method compares with other method
| Method | Detection limit (μ g L -1) | Sample volume (mL) | Extraction time (min) |
| DLLME-HPLC-UV | 0.07 | 10 | 3 |
| SPME-HPLC-FLD | 0.43 | 10 | 60 |
| SPME-HPLC-UV | 0.1 | 1 | 35 |
| SPME-HPLC-FLD | 0.02 | 4 | 25 |
| VALLME-HPLC-UV | 0.02 | 20 | 2 |
| VALLME-HPLC-FLD | 0.02 | 5 | 1.5 |
Note DLLME: be dispersive liquid-liquid microextraction; SPME: solid-phase microextraction; VALLME: be the inventive method; HPLC: be high performance liquid chromatography; UV: be UV-detector; FLD: be fluorescence detector.
After the former water high-efficient liquid phase chromatogram of river and mark-on, high-efficient liquid phase chromatogram is shown in Fig. 3.It can thus be appreciated that the inventive method can divide bisphenol-A in bleed by the quick ﹑ of fast fast ﹑ spirit fast exactly.
Claims (2)
1., without condensation and the method for melting collection extractant mensuration bisphenol-A again, it is characterized in that, comprise step:
(1) based on the vortex auxiliary liquid phase extraction of extractant gathering-device: utilize extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize turbula shaker to carry out vortex to water sample and extractant system, extractant is broken for the vortex auxiliary liquid phase extraction that fine drop accelerates rate of extraction;
(2) based on the detection of the bisphenol-A of high performance liquid chromatography-fluorescence device: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283nm, emission wavelength 323nm; Liquid phase chromatogram condition is: liquid-phase chromatographic column is 250mm × 4.6mm, the C18 chromatographic column of 5 μm, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is become 7:3 in 5:5,15min, flow rate of mobile phase 1.0mLmin
-1.
2. method according to claim 1, it is characterized in that, the described extractant gathering-device of step (1) is made up of the first glass tube and the second glass tube, water sample to be determined contained by second glass tube, and two ends internal diameter is identical, and the first glass tube two ends internal diameter has a long way to go, butt end external diameter is slightly less than the internal diameter of the second glass tube, just cover water sample liquid level above the second glass tube, taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001337080A (en) * | 2000-05-30 | 2001-12-07 | Asahi Kasei Corp | Phenols analyzing method |
| CN102680604A (en) * | 2012-05-30 | 2012-09-19 | 天津春宇食品配料有限公司 | Pretreatment method and detection method for bisphenol A in water samples and plastic products |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001337080A (en) * | 2000-05-30 | 2001-12-07 | Asahi Kasei Corp | Phenols analyzing method |
| CN102680604A (en) * | 2012-05-30 | 2012-09-19 | 天津春宇食品配料有限公司 | Pretreatment method and detection method for bisphenol A in water samples and plastic products |
Non-Patent Citations (5)
| Title |
|---|
| Dispersive liquid–liquid microextraction combined with high-performance liquid chromatography-UV detection as a very simple, rapid and sensitive method for the determination of bisphenol A in water samples;Mohammad Rezaee等;《Journal of Chromatography A》;20091231;第1216卷;第1511-1514页 * |
| 分散液-液微萃取 /高效液相色谱法测定水样中的痕量双酚A;李鱼等;《高等学校化学学报》;20081130;第29卷(第11期);第2143页第1节 * |
| 分散液-液微萃取-高效液相色谱法测定环境水样中的多环芳烃;张建华等;《色谱》;20091130;第27卷(第6期);第799-803页 * |
| 固相萃取-高效液相色谱-荧光检测法同时测定水中的壬基酚和双酚A;王晓东等;《分析试验室》;20060930;第25卷(第9期);第27-29页 * |
| 高效液相色谱-串联质谱法测定环境水体中双酚 A、辛基酚、壬基酚;张奎文等;《分析试验室》;20080831;第27卷(第8期);第62-66页 * |
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