CN107245334A - A kind of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion and preparation method thereof - Google Patents
A kind of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to a kind of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion and preparation method thereof, structural formula is：Preparation method：Acid binding agent is added in luciferin solution, ice-water bath cooling adds acryloyl chloride solution; 23~25h is reacted at room temperature, solvent, vacuum drying is removed; obtain acryloyl group fluorescein; it is then dissolved in solvent, hydrazine hydrate solution, 75~80 DEG C of 10 14h of reaction is added dropwise; remove solvent and unreacted hydrazine hydrate; recrystallization, dries, obtains ACFH；ACFH, acrylamide and AIBN are dissolved in solvent, are placed in ampoule bottle, bottle is sealed after the logical 30min of high pure nitrogen 15,70 80 DEG C of 8~15h of reaction, suction filtration is purified, is dried in vacuo, and grinding is produced.The fluorescent probe compounds of the present invention have good selectivity to mercury ion, and applied in the aqueous solution, not only facilitate but also with preferable using effect in environmental applications.
Description
Technical field
The invention belongs to fluorescence probe material and its field processed, more particularly to a kind of water soluble polymer for detecting mercury ion
Fluoresceins fluorescence probe and preparation method thereof.
Background technology
Mercury is one of high and generally existing heavy metal element of nature Poisoning.It is widely distributed in us per born
In product needed for work, for example：Battery, printing and electronic equipment etc..Mercury element and mercury ion can by the bacterium in environment
To change into methyl mercury, then added up by food chain in organism, the meeting under conditions of low concentration due to methyl mercury
There are very high affinity, therefore the serious health problem that have impact on people to the thiol group and enzyme in protein.Therefore, in life
Development is in real time in terms of the fields such as thing, environment and diagnosis monitoring and quick detection mercury ion turns into our active demand.Currently, often
The mercury element detection means seen is mainly Atomic absorption/emission spectrometry, gas chromatography, nuclear magnetic resonance, X-ray fluorescence spectra
Method, inductively coupled plasma mass spectrometry, electrochemical method (such as anodic stripping voltammetry, redox potentiometry), colorimetric method
(such as traditional dithizone method).Traditional means of testing is cumbersome and equipment is expensive and can not continuously be monitored.This
In the case of traditional technology can not meet, we are in the urgent need to finding other detection means.In the nearest more than ten years, find
Fluorescence probe detection method has convenience good, the high advantage of selectivity, sensitivity, there is many on small molecule fluorescent spy in recent years
The skill of handling needles detects the report of mercury ion, Chinese patent 201310163699.9 " mercury ion fluorescent sensor and its synthetic method and should
With ", the reaction generation rhodamine acid amides by raw material of rhodamine B and hydrazine hydrate, then add isocyanates reaction synthesis mercury from
The Fluorescence Fluorescence sensor of son；Chinese patent 201410029789.3 is " a kind of to be used to detect metal ion content in water environment
Organic compound and its application ", with N- [2- ((alkyl mercapto ethyl) the aminobenzene oxygen of N ' N '-two ethyl]-N- alkyl mercapto ethyls -2-
Alkoxyl aniline is used as ion complexation body, it is adaptable to the continuous detection of various Metals in Environments ion concentrations, especially to mercury ion
Detection.Fluorescence property of the fluorescein with uniqueness, its detection optical wavelength (λ ex) and wavelength of transmitted light (λ em) are respectively positioned on visible
Light area, the loss for preventing ultraviolet light from being caused to cell, and fluorescence quantum yield are high；Easily with some biomolecule with covalent bond or non-
The form of covalent bond combines to form label or compound；Nontoxic, cost is low.Therefore have in terms of fluorescence probe is developed important
Application prospect.Chinese patent " the response type fluoresceins fluorescence probe of detection mercury ion and its preparation of applicant's early stage application
With applying (Chinese patent 105924449A) ", it is 445nm, detection in excitation wavelength using fluorescent spectrometry in aqueous
Launch wavelength is 512nm, detect mercury ion concentration 0.1-10nM scope reach one very well it is linear, detection is limited to
0.4nM, mercury ion solution is detected using fluorescence probe method, can be achieved to the real-time of mercury ion and quick detection, environment with
There is preferable application prospect in terms of biological detection.However, the report of water-soluble high sensitivity macromolecule mercury ion fluorescence probe compared with
It is few.
The content of the invention
It is glimmering that the technical problems to be solved by the invention are to provide a kind of water soluble polymer fluoresceins for detecting mercury ion
Light probe and preparation method thereof, the fluorescence probe has good selectivity to mercury ion in aqueous, in environment measuring and life
Object space face has preferable application prospect.
A kind of water soluble polymer fluoresceins fluorescence probe of detection mercury ion of the present invention, structural formula is：Wherein, n is the integer in 10~50；M is whole in 300-1000
Number.
A kind of preparation method of the water soluble polymer fluoresceins fluorescence probe of detection mercury ion of the present invention, including：
(1) acid binding agent is added in luciferin solution, then ice-water bath cooling adds acryloyl chloride solution, room temperature is anti-
23~25h is answered, solvent is removed, vacuum drying obtains acryloyl group fluorescein；
(2) the acryloyl group fluorescein obtained in step (1) is dissolved in solvent, hydrazine hydrate solution, 75~80 DEG C is added dropwise
10-14h is reacted, solvent and unreacted hydrazine hydrate is removed, recrystallized, dries, obtains acryloyl chloride fluorescein hydrazides ACFH；
(3) ACFH in step (2), acrylamide and azodiisobutyronitrile AIBN are dissolved in solvent, obtain mixing molten
Liquid；Then mixed solution is placed in container in (preferably ampoule bottle), leads to after high pure nitrogen 15-30min and seal (envelope bottle), 70-
80 DEG C of 8~15h of reaction (in course of reaction it can be seen that having sediment precipitation in reaction bulb), suction filtration (obtains yellow solid), purification,
Vacuum drying, grinding obtains detecting the water soluble polymer fluoresceins fluorescence probe (yellow powder PAFM) of mercury ion.
Acid binding agent is the organic amine alkaline reagents such as triethylamine, diethylamine in the step (1).
The structural formula of fluorescein is in the step (1)：
The concentration of luciferin solution is 0.45~0.5mol/L in the step (1), and solvent is C2H4C12；Acryloyl chloride is molten
The concentration of liquid is 5.5~6mol/L, and solvent is C2H4C12。
The mol ratio of fluorescein, acid binding agent and acryloyl chloride is 1 in the step (1)：2~2.5：1~1.5.
The method that solvent is removed in the step (1) is rotary evaporation, and condition is：The temperature of rotary evaporation is 20~30
DEG C, vacuum is 101~105KPa, and the time is 0.5~1h.
In the step (1) reaction process is tracked by using TCL plates.
The mol ratio of acryloyl group fluorescein and hydrazine hydrate is 1 in the step (2)：1~6.
Solvent is absolute ethyl alcohol in the step (2)；The mass fraction of hydrazine hydrate solution is 80%.
The method that solvent and unreacted hydrazine hydrate are removed in the step (2) is rotary evaporation, and condition is：Rotary evaporation
Temperature be 50~60 DEG C, vacuum be 101~105KPa, the time be 1~2h.
Recrystallization is using tetrahydrofuran recrystallization in the step (2).
ACFH, acrylamide and AIBN mol ratio are 1 in the step (3)：40~60：0.05~0.3.
Solvent is tetrahydrofuran in the step (3).
The operation of purification is in the step (3)：The solid filter paper parcel that suction filtration is obtained is placed in apparatus,Soxhlet's,
Solvent extraction is made of tetrahydrofuran to remove oligomer or unreacted monomer.
It is described detection mercury ion water soluble polymer fluoresceins fluorescence probe apply detection the aqueous solution in mercury from
In son.
Fluorescence probe PAFM autofluorescences of the present invention are very weak, are dissolved in after being mixed after the aqueous solution with mercury ion, produce
Strong fluorescence, under conditions of mercury ion, by 460nm excited by visible light, the fluorescence signal at 515nm is significantly increased, and is led to
Overwriting fluorescence intensity is the concentration of detectable mercury ion.Fluorescence probe ACFH can to mercury ion in pH=7 cushioning liquid
Carry out high selectivity detection.The fluorescence intensity of described fluorescence probe, into good linear relationship, is quantitatively examined with ion concentration of mercury
The range of linearity for surveying ion concentration of mercury is 1-10nM, and lowest detection is limited to 0.35nM.
The syntheti c route of the fluorescence probe of the present invention is as follows：
More preferable detection sensitivity is presented and bigger in the water-soluble high sensitivity macromolecule mercury ion fluorescence probe of the present invention
Complexation constant, while propionamide macromolecule medium has fine biocompatibility, biodegradation and Premeabilisation of cells performance, it is expected to
Biological imaging and disease detection etc. have more preferable application prospect.
Beneficial effect
(1) water soluble polymer fluorescent probe compounds of the invention have good selectivity to mercury ion, and apply
In the aqueous solution, not only facilitate but also with preferable using effect in environmental applications；
(2) fluorescent probe compounds of the invention are solid powder, are easy to use storage, and synthetic method is simple, receive
Rate is high, cost is low, and application prospect is good.
Brief description of the drawings
Fig. 1 is the ultraviolet change collection of illustrative plates that fluorescence probe is added before and after mercury ion；Abscissa is UV absorption wavelength (nm), is indulged
Coordinate is absorbance；
Fig. 2 is that fluorescence probe adds fluorescence excitation and transmitting collection of illustrative plates after mercury ion；Abscissa is fluorescence emission wavelengths (nm),
Ordinate is fluorescence intensity；
Fig. 3 be concentration be 0.35nM probe solution using Britton-Robinson cushioning liquid be configured with it is a series of not
With pH cushioning liquid, the optimal pH of detection probe and ion complexation；Abscissa is pH, and ordinate is fluorescence intensity；
Fig. 4 is that fluorescence probe concentration is 0.35nM in aqueous to different metal ion (Cd2+、Al3+、Cu2+、Co2+、
Sn2+、Ca2+、Fe3+、Zn2+、Ba2+、Mg2+、Pb2+、Bi+) selection interference detection fluorescence response figure；Abscissa is different gold
Belong to ion, ordinate is fluorescence intensity；
Fig. 5 is the Job-Plot curves that fluorescence probe concentration 0.35nM is complexed ratio with mercury ion；Abscissa is c [Hg2+]/c
[Hg2++ probe], ordinate is fluorescence F-F0, wherein F, F0It is the fluorescent emission intensity in 460nm；
Fig. 6 is that fluorescence probe concentration is fluorescence spectrum response diagrams of the 3.5nM in aqueous to mercury ion；Abscissa is glimmering
Light launch wavelength (nm), ordinate is fluorescence intensity；Each curve Hg in Fig. 62+Concentration be 0,4 × 10 successively from low to high- 10Mol/L, 8 × 10-10Mol/L, 2 × 10-9Mol/L, 3 × 10-9Mol/L, 4 × 10-9Mol/L, 8 × 10-9Mol/L, 10-8mol/
L, 3 × 10-8Mol/L, 5 × 10-8Mol/L, 7 × 10-8Mol/L, 9 × 10-8Mol/L, 2 × 10-7Mol/L, 5 × 10-7Mol/L,
10-6Mol/L, 10-5Mol/L, 1.5 × 10-5Mol/L, 2 × 10-5mol/L；
Fig. 7 is that fluorescence probe concentration is that fluorescence of the 0.35nM in aqueous to various concentrations mercury ion at 515nm is strong
Degree；Abscissa is the concentration 10 of mercury ion-5M, ordinate is fluorescence intensity；
Fig. 8 is that fluorescence probe concentration is that 0.35nM schemes to the fluorescence spectrum response time of mercury ion in aqueous；It is horizontal to sit
The response time (min) is designated as, ordinate is fluorescence intensity；
Embodiment
With reference to specific embodiment, the present invention is expanded on further.It should be understood that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, people in the art
Member can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Scope.
Embodiment 1
The detection mercury ion water soluble polymer fluoresceins fluorescence probe of the present embodiment, its structural formula is：
N=291, m=9.
The preparation method of the plain class fluorescence probe of above-mentioned detection mercury ion reactive type water-solubility high molecular fluorescent is：
(1) 3.00g (9.0 × 10 is accurately weighed-3Mol) fluorescein powder (fluorescein is commercially available prod) is placed in equipped with temperature
In the 100mL flask with three necks,round bottom of degree meter and condenser pipe, the C for taking 20.0mL to dry with graduated cylinder2H4C12Fluorescein powder is dissolved
Obtain luciferin solution, then add acid binding agent of 3.0mL (0.02mol) triethylamines as reaction, magnetic agitation；It is secondary anti-to reduce
Should, by the mixed liquor of gained in -2 DEG C~3 DEG C ice-water baths it is sufficiently cool, take 1.00g (1.1 × 10-2Mol) acryloyl chloride is dissolved in
20.0mL C2H4C12In obtain acryloyl chloride solution, be slowly dropped in 30min in above-mentioned mixed liquor；Treat acryloyl
After the dichloromethane solution of chlorine is dripped, ice-water bath is removed, makes mixed liquor that reaction 24h is stirred at room temperature, passes through a thin layer
Chromatosheet monitors reaction process, by with different volumes than chloroform/ethanol mixed liquor point plate compare the Rf value of reaction product,
Finally select volume ratio 1:30 chloroform/ethanol mixed liquor is used as solvent.Terminate after reaction, be 25 DEG C, vacuum in temperature
Partial solvent, which is removed, for rotary evaporation 1h under conditions of 101KPa obtains orange colour mixture.It is 101KPa in 45 DEG C, vacuum
Under conditions of be dried in vacuo 8 hours, finally give bright yellow solid 3- acryloyl group fluoresceins.
(2) 3- acryloyl groups fluorescein (0.373g, 1.0mmol) is dissolved in 20mL absolute ethyl alcohols, 80% water is added dropwise
Hydrazine solution (0.3mL, 5.7mmol) is closed, control temperature is in 79 DEG C of heating reflux reaction 12h.Temperature be 55 DEG C, vacuum be
Rotary evaporation 1h removes solvent and unreacted hydrazine hydrate, product tetrahydrofuran repeated recrystallize, mistake under conditions of 101KPa
Filter, is dried to obtain flaxen acryloyl chloride fluorescein hydrazides (ACFH).FTIR(KBr):ν=3418cm-1(-NH2),
1681cm-1(C=O), 1614cm-1,1503cm-1,1447cm-1, (C=C), 2927cm-1(Ar-H),1175cm-1(C-O),
1111cm-1(C-H in-plane bending)1HNMR(400MHz,CDCl3):6.44 (s, 1H ,=CH2),6.65-8.02(m,10H,
Ar-H)。
(3) first by 3.50 × 10-2g(1.4×10-4MoL) acryloyl group fluorescein hydrazides (ACFH), 0.5000g (7.0 ×
10-3MoL) acrylamide (AM) and 3.1 × 10-3G azodiisobutyronitriles AIBN (1.9 × 10-5MoL 10.0mL tetrahydrochysenes) are dissolved in
In furans, then mixed solution is placed in dry ampoule bottle, logical high pure nitrogen seals bottle, 70 DEG C of reaction 10h of constant temperature after 15 minutes.
It can be seen that having sediment precipitation in reaction bulb in course of reaction.Stop after reaction, suction filtration reactant mixture can obtain yellow solid.Will
Solid filter paper that suction filtration is obtained parcel is placed in apparatus,Soxhlet's, and solvent extraction is made of tetrahydrofuran to remove oligomer or not
The monomer of reaction, by vacuum drying, grinding obtains yellow powder fluorescence probe (PAFM), i.e., above-mentioned detection mercury ion reaction
Type fluoresceins fluorescence probe.FTIR(KBr):ν=3418cm-1(-NH2),1681cm-1(C=O), 1614cm-1,1503cm-1,
1447cm-1(C=C), 2927cm-1(Ar-H),1175cm-1(C-O),1111cm-1(C-H in-plane bending), 1700cm-1(O-C
=O), 1537cm-1(C-N).1HNMR(400MHz,CDCl3):6.44 (s, 1H ,=CH2),6.65-8.02(m,10H,Ar-H),
4.37(m,4H,-NH2), 2.18 (m, 10H, CH2)。
Embodiment 2
Ion is carried out using the detection mercury ion reactive type water-solubility high molecular fluorescent plain class fluorescence probe in embodiment 1
Detection：
Fig. 1 is the ultraviolet change collection of illustrative plates that fluorescence probe is added before and after mercury ion, as can be seen from the figure：Probe molecule PAFM
No ultraviolet absorption peak at 400-500nm itself, probe at 462nm and 495nm with after mercury ion complexing, occurring two
Absworption peak.
Fig. 2 is that fluorescence probe adds fluorescence excitation and transmitting collection of illustrative plates after mercury ion, as can be seen from the figure：Fluorescence probe with
Fluorescence exciting wavelength is 460nm after mercury ion complexing, and fluorescence emission wavelengths are 515nm.
Fig. 3 be concentration be 0.35nM probe solution using Britton-Robinson cushioning liquid be configured with it is a series of not
With pH cushioning liquid, the optimal pH of detection probe and ion complexation.As shown in figure 3, gained is detected into the anti-of mercury ion
Answer type fluoresceins fluorescence probe to be dissolved in and 10 μM of probe solution is made into aqueous solvent, add Britton-Robinson bufferings molten
Liquid be configured with it is a series of it is different (pH=2.18,3.15,4.09,4.64,5.96,6.55,7.0,8.77,8.90,9.56,
11.07th, 11.58,12.01) pH cushioning liquid, it is 1x10 that 1mL concentration is then added into probe solution-4MM mercury ion,
Detect the change of probe solution fluorescence intensity under condition of different pH.It was found that fluorescence intensity is most strong when pH=7 or so, therefore
The fluorescence probe is in aqueous solvent, and in pH=7 or so, probe solution is stable is conducive to detection.
As shown in figure 4, being Hg2+Fluorescence titration experiment to PAFM solution, to common metal ion Cd2+、Al3+、Cu2+、
Co2+、Sn2+、Ca2+、Fe3+、Zn2+、Ba2+、Mg2+、Pb2+、Bi+Fluorescence titration is carried out.Fluorescence probe ACFH is dissolved in water-soluble
In agent, 0.35nM fluorescence probe solution is made into, respectively by HgCl2、CdCl2、Al2(SO4)3、CuSO4、CoCl2、SnCl2、CaCl2、
FeCl3、Zn(NO3)2、BaCl2、MgSO4、Pb(NO3)2、BiNO3It is dissolved in aqueous solvent, is made into 10nM Hg2+、Cd2+、Al3+、Cu2 +、Co2+、Sn2+、Ca2+、Fe3+、Zn2+、Ba2+、Mg2+、Pb2+、Bi+Metal ion solution, carries out selection interference detection.Excitation wave
Under conditions of a length of 460nm, the fluorescence intensity that detection launch wavelength is 515nm；Solid post is that fluorescence probe PAFM concentration is
0.35nM, respectively to metal ion (10-7M)Cd2+、Al3+、Cu2+、Co2+、Sn2+、Ca2+、Fe3+、Zn2+、Ba2+、Mg2+、Pb2+、Bi+The fluorescence intensity of fluorescence titration is carried out, open tubular column is in PAFM-Hg2+(10-5M metal ion (10) is separately added into system- 5M)Cd2+、Al3+、Cu2+、Co2+、Sn2+、Ca2+、Fe3+、Zn2+、Ba2+、Mg2+、Pb2+、Bi+The fluorescence for having carried out fluorescence titration is strong
Degree.
As shown in figure 5, fixed fluorescence probe and Hg2+Concentration summation be 50nM, by changing the concentration ratio (fluorescence of the two
Probe and the ratio of mercury ion amount of substance are followed successively by 10：0,9：1,8：2,7：3,6：4,5：5,4：6,3：7,2：8,1：9,0：10)
The difference of fluorescence intensity and fluorescence probe autofluorescence intensity under the concentration to 515nm, the ratio of total concentration is accounted for ion
Make Fig. 5.Understand to work as Hg by this figure2+Proportion be 0.5 when ordinate can reach peak, it may be determined that fluorescence probe with
Hg2+Between it is main with 1:1 form combines to form stable compound.
As shown in figure 5, probe molecule PAFM (0.35nM) is having other ions, (ion concentration is (10-7When M)), remove
Hg2+Outside, fluorescence intensity is added after other metal ions in PAFM solution without significant change.In disturbed test, other ions
Addition to PAFM-Hg2+The influence of the fluorescence intensity of complex system is nor very big.Illustrate PAFM and Hg2+Stabilization can be formed
Complex compound.
As shown in fig. 6, when adding various concentrations mercury ion into fluorescence probe (0.35nM) solution, fluorescence probe solution is glimmering
Light luminescent spectrum, emission peak is in 515nm.
As shown in fig. 7, solution at 515nm fluorescent emission peak intensity with add Hg2+The increase fluorescence of ion concentration is strong
Degree change.Work as Hg2+When ion concentration reaches 10nM, the fluorescence intensity of ligand fluorescence probe is almost no longer with the increase of ion concentration
And change.
As shown in figure 8, the response time is to PAFM-Hg2+Fluorescence intensity influence, when adding finite concentration in PAFM solution
Hg2+Afterwards, the fluorescence intensity of its compound constantly changes with the increase of time.Thus, it can be seen that during optimal solution detection stabilization
Between be 3min.
Claims (10)
1. a kind of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion, it is characterised in that：Structural formula is：Wherein, n is the integer in 10~50；M is whole in 300-1000
Number.
2. a kind of preparation method for the water soluble polymer fluoresceins fluorescence probe for detecting mercury ion, including：
(1) acid binding agent is added in luciferin solution, then ice-water bath cooling adds acryloyl chloride solution, room temperature reaction 23
~25h, removes solvent, and vacuum drying obtains acryloyl group fluorescein；
(2) the acryloyl group fluorescein obtained in step (1) is dissolved in solvent, hydrazine hydrate solution, 75~80 DEG C of reactions is added dropwise
10-14h, removes solvent and unreacted hydrazine hydrate, recrystallizes, and dries, obtains acryloyl chloride fluorescein hydrazides ACFH；
(3) ACFH in step (2), acrylamide and azodiisobutyronitrile AIBN are dissolved in solvent, obtain mixed solution；So
Mixed solution is placed in container afterwards, leads to after high pure nitrogen 15-30min and seals, 70-80 DEG C of 8~15h of reaction, suction filtration, purification,
Vacuum drying, grinding obtains detecting the water soluble polymer fluoresceins fluorescence probe of mercury ion.
3. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that acid binding agent is triethylamine or diethylamine in the step (1).
4. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that the structural formula of fluorescein is in the step (1)：
5. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that the concentration of luciferin solution is 0.45~0.5mol/L in the step (1), and solvent is C2H4C12；Propylene
The concentration of solution of acid chloride is 5.5~6mol/L, and solvent is C2H4C12。
6. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that the mol ratio of fluorescein, acid binding agent and acryloyl chloride is 1 in the step (1)：2~2.5：1~1.5.
7. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that the mol ratio of acryloyl group fluorescein and hydrazine hydrate is 1 in the step (2):1~6.
8. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that solvent is absolute ethyl alcohol in the step (2)；The mass fraction of hydrazine hydrate solution is 80%.
9. a kind of preparation side of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that ACFH, acrylamide and AIBN mol ratio are 1 in the step (3)：40~60：0.05~0.3.
10. a kind of preparation of water soluble polymer fluoresceins fluorescence probe for detecting mercury ion according to claim 2
Method, it is characterised in that solvent is tetrahydrofuran in the step (3).
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