CN103954703A - Method for determining bisphenol A without condensing and remelting for collecting extraction agent - Google Patents
Method for determining bisphenol A without condensing and remelting for collecting extraction agent Download PDFInfo
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- CN103954703A CN103954703A CN201410164857.7A CN201410164857A CN103954703A CN 103954703 A CN103954703 A CN 103954703A CN 201410164857 A CN201410164857 A CN 201410164857A CN 103954703 A CN103954703 A CN 103954703A
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Abstract
The invention discloses a method for determining bisphenol A without condensing and remelting for collecting an extraction agent. The method comprises the following steps: (1) carrying out vortex-assisted liquid-phase micro-extraction based on an extraction agent collecting device; and (2) detecting bisphenol A based on a high performance liquid chromatography-fluorescence detector. A technical scheme for collecting trace extraction agent by use of the extraction agent collecting device is provided firstly, the condensing and the melting steps are eliminated, the separation and concentration efficiency of the bisphenol A in water can be improved, and the analysis is accelerated. The method has the advantages of rapidness, sensitivity, accuracy, environment friendliness and the like.
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 is taking vortex liquid-phase micro-extraction as 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 is 2,700 ten thousand tons of plastics that contain bisphenol-A of annual production now, 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 including water body to have it to detect.Numerous research datas are verified, and bisphenol-A can cause endocrinopathy, are a kind of incretion interferents, can serious threat fetus and children healthy.Separately have data to show, the obesity that cancer and metabolic disturbance cause is also polluted and is had substantial connection with bisphenol-A.
In water body, the detection of bisphenol-A has more report, comprises that the instruments such as gas chromatography-mass spectrometry (GC/MS), gas chromatography-tandem mass spectrum coupling (GC/MS/MS), liquid chromatography-mass spectrometry (LC/MS), liquid chromatography-tandem mass spectrum coupling (LC/MS/MS) are 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, has obtained analytical work person and has more and more favored.And in dispersive liquid-liquid microextraction, because the toxicity of the little organic solvent of the density ratio water organic solvent large compared with density ratio water is little, analytical work person is healthy for protection, be more prone to use organic solvent that density ratio water is little as extractant.In the time using the little extractant of density ratio water, 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 in bisphenol-A mensuration process liquid-phase micro-extraction pre-treatment step more, the problem that analysis efficiency is lower, provides a kind of without condensation with melt and collect the device of extractant and for bisphenol-A method for measuring.
Technical scheme of the present invention is as follows:
Without condensation with melt and collect extractant and measure the method for bisphenol-A, it comprises step:
(1) the auxiliary liquid-phase micro-extraction of the vortex based on extractant gathering-device;
(2) detection of the bisphenol-A based on high performance liquid chromatography-fluorescence detector.
Foregoing method, preferred scheme is, the auxiliary liquid-phase micro-extraction of the vortex of step (1) based on extractant gathering-device is to utilize extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize vortex a pair of oscillators water sample and extractant system to carry out vortex, extractant is broken for to the auxiliary liquid-phase micro-extraction of vortex of fine drop quickening rate of extraction.
Foregoing method, preferred scheme is, described extractant gathering-device is made up of glass tube (1) and glass tube (2), glass tube (2) is contained water sample to be determined, 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, preferably scheme is, the detection of the bisphenol-A of step (2) based on high performance liquid chromatography-fluorescence detector: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283 nm, emission wavelength 323 nm.
Foregoing method, preferably scheme is, liquid-phase chromatographic column C18 (250 mm × 4.6 mm, m) chromatographic column of 5 μ, mobile phase acetonitrile and water, gradient elution, start acetonitrile: water is 5:5, in 15 min, becomes 7:3, flow rate of mobile phase 1.0 mL min
-1.
The analytical approach of bisphenol-A in a kind of water provided by the invention, taking method is the detection of the bisphenol-A of the auxiliary liquid-phase micro-extraction (2) of (1) vortex based on extractant gathering-device based on high performance liquid chromatography-fluorescence detector.In described step (1), extractant gathering-device is shown in Fig. 1, is made up of glass tube 1 and glass tube 2, and 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 glass tube 2 top water sample liquid levels, 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 vortex a pair of oscillators water sample and extractant system to carry out vortex, extractant is broken for to fine drop and accelerates rate of extraction.In described step (1), extraction drop little density ratio water is covered on to glass tube 1 larger one end of internal diameter, slow decreasing glass tube, 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 of having collected.In described step (2), bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283 nm, emission wavelength 323 nm.In described step (2), liquid phase chromatogram condition is: liquid-phase chromatographic column C18 (250 mm × 4.6 mm, m) chromatographic column of 5 μ, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is 5:5, in 15 min, become 7:3, flow rate of mobile phase 1.0 mL min
-1.
Beneficial effect of the present invention is: Ke is with the bisphenol-A in Kuai Su ﹑ sensitive analysis water.This method proposes a kind of scheme of utilizing extractant gathering-device to collect micro-extractant 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.
Brief description of the drawings
Fig. 1 is extractant gathering-device structural representation.
Fig. 2 is bisphenol-A analyzing and testing process flow diagram.
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) the auxiliary liquid-phase micro-extraction of the vortex based on extractant gathering-device: utilize extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize vortex a pair of oscillators water sample and extractant system to carry out vortex, extractant is broken for to the auxiliary liquid-phase micro-extraction of vortex of fine drop quickening rate of extraction; Described extractant gathering-device is made up of glass tube 1 and glass tube 2, glass tube 2 is contained water sample to be determined, 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 glass tube 2 top water sample liquid levels, taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle.
(2) detection of the bisphenol-A based on high performance liquid chromatography-fluorescence detector: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283 nm, emission wavelength 323 nm.Liquid phase chromatogram condition is: and liquid-phase chromatographic column C18 (250 mm × 4.6 mm, m) chromatographic column of 5 μ, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is 5:5, in 15 min, becomes 7:3, flow rate of mobile phase 1.0 mL min
-1.
The analytical approach of bisphenol-A in the former water of embodiment 2 certain river, taking method is the auxiliary liquid-phase micro-extraction separation and concentration bisphenol-A of (1) vortex based on extractant gathering-device, the detection of (2) bisphenol-A based on high performance liquid chromatography-fluorescence detector.
(1) based on the auxiliary liquid-phase micro-extraction separation and concentration bisphenol-A of the vortex of extractant gathering-device: get the water that 5 mL contain bisphenol-A and be placed in glass test tube, add 30 μ L isooctyl alcohol extractants, utilize vortex oscillator to carry out the vortex auxiliary extraction of water, coextraction 90 s.When vortex extraction, in water, bisphenol-A is extracted in isooctyl alcohol.After extraction, place 2 min, 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 as shown in Figure 1 extractant gathering-device, glass tube 2 is contained water sample to be determined, 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 glass tube 2 top water sample liquid levels, taper end internal diameter is very thin, can just insert micro-sampling pin syringe needle), glass device 1 is covered on to liquid level top in glass device 2, and extraction drop is covered on to the inside.Glass device 1 is highly slowly declined, and extract dropping liquid face slowly rises in glass device 1.Because glass device 2 two ends internal diameters have a long way to go, isooctyl alcohol, at the larger liquid level of the most advanced and sophisticated height of formation of glass device 2, is directly drawn 10 μ L isooctyl alcohol with micro-sampling pin and is carried out the analysis of liquid chromatography-fluorescence detector.Whole analytic process as shown in Figure 2.
(2) detection of the bisphenol-A based on high performance liquid chromatography-fluorescence detector: high efficiency liquid phase system, be furnished with fluorescence and UV-detector.When fluoroscopic examination, fluorescence detector excitation wavelength 283 nm, bisphenol-A emission wavelength 323 nm.Liquid-phase chromatographic column is that (mobile phase is acetonitrile and water to C18 for 250 mm × 4.6 mm, m) chromatographic column of 5 μ, and gradient elution starts acetonitrile: water is 5:5, in 15 min, becomes 7:3, flow rate of mobile phase 1.0 mL min
-1.
Table 1 is the correlation data of this method and other method.
The comparison of table 1 this method and 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.Hence one can see that, and the inventive method fast quick ﹑ of fast fast ﹑ spirit is divided bisphenol-A in bleed exactly.
Claims (5)
1. without condensation with melt again and collect extractant and measure the method for bisphenol-A, it is characterized in that, comprise step:
(1) the auxiliary liquid-phase micro-extraction of the vortex based on extractant gathering-device;
(2) detection of the bisphenol-A based on high performance liquid chromatography-fluorescence detector.
2. method according to claim 1, it is characterized in that, the auxiliary liquid-phase micro-extraction of the vortex of step (1) based on extractant gathering-device is to utilize extractant gathering-device, using micro-isooctyl alcohol as extractant, utilize vortex a pair of oscillators water sample and extractant system to carry out vortex, extractant is broken for to the auxiliary liquid-phase micro-extraction of vortex of fine drop quickening rate of extraction.
3. method according to claim 2, it is characterized in that, described extractant gathering-device is made up of glass tube (1) and glass tube (2), glass tube (2) is contained water sample to be determined, 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.
4. method according to claim 1, it is characterized in that the detection of the bisphenol-A of step (2) based on high performance liquid chromatography-fluorescence detector: bisphenol-A analytic system is high performance liquid chromatograph, is furnished with fluorescence detector, fluorescence detector excitation wavelength 283 nm, emission wavelength 323 nm.
5. method according to claim 4, it is characterized in that, liquid phase chromatogram condition is: liquid-phase chromatographic column C18 (250 mm × 4.6 mm, m) chromatographic column of 5 μ, mobile phase acetonitrile and water, gradient elution, starts acetonitrile: water is 5:5, in 15 min, become 7:3, flow rate of mobile phase 1.0 mL min
-1.
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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 |
|---|
| MOHAMMAD REZAEE等: "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", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| 张奎文等: "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", 《分析试验室》 * |
| 张建华等: "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", 《色谱》 * |
| 李鱼等: "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", 《高等学校化学学报》 * |
| 王晓东等: "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", 《分析试验室》 * |
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