CN110108809A - A kind of measuring method of essence crudefiber crop drug - Google Patents
A kind of measuring method of essence crudefiber crop drug Download PDFInfo
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- CN110108809A CN110108809A CN201910352758.4A CN201910352758A CN110108809A CN 110108809 A CN110108809 A CN 110108809A CN 201910352758 A CN201910352758 A CN 201910352758A CN 110108809 A CN110108809 A CN 110108809A
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- crudefiber crop
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- 239000003814 drug Substances 0.000 title claims abstract description 110
- 229940079593 drug Drugs 0.000 title claims abstract description 102
- 238000000034 method Methods 0.000 title claims abstract description 38
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 39
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- 238000010828 elution Methods 0.000 claims description 24
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 23
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- 239000011159 matrix material Substances 0.000 claims description 7
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- 239000000843 powder Substances 0.000 claims description 7
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- 229940049706 benzodiazepine Drugs 0.000 claims description 5
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- RGCVKNLCSQQDEP-UHFFFAOYSA-N Perphenazine Chemical compound C1CN(CCO)CCN1CCCN1C2=CC(Cl)=CC=C2SC2=CC=CC=C21 RGCVKNLCSQQDEP-UHFFFAOYSA-N 0.000 claims description 3
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- 229960000836 amitriptyline Drugs 0.000 claims description 3
- KRMDCWKBEZIMAB-UHFFFAOYSA-N amitriptyline Chemical compound C1CC2=CC=CC=C2C(=CCCN(C)C)C2=CC=CC=C21 KRMDCWKBEZIMAB-UHFFFAOYSA-N 0.000 claims description 3
- 229960001657 chlorpromazine hydrochloride Drugs 0.000 claims description 3
- 229960003529 diazepam Drugs 0.000 claims description 3
- AAOVKJBEBIDNHE-UHFFFAOYSA-N diazepam Chemical compound N=1CC(=O)N(C)C2=CC=C(Cl)C=C2C=1C1=CC=CC=C1 AAOVKJBEBIDNHE-UHFFFAOYSA-N 0.000 claims description 3
- CDCHDCWJMGXXRH-UHFFFAOYSA-N estazolam Chemical compound C=1C(Cl)=CC=C(N2C=NN=C2CN=2)C=1C=2C1=CC=CC=C1 CDCHDCWJMGXXRH-UHFFFAOYSA-N 0.000 claims description 3
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- RONZAEMNMFQXRA-UHFFFAOYSA-N mirtazapine Chemical compound C1C2=CC=CN=C2N2CCN(C)CC2C2=CC=CC=C21 RONZAEMNMFQXRA-UHFFFAOYSA-N 0.000 claims description 3
- 229960001785 mirtazapine Drugs 0.000 claims description 3
- 229960004535 oxazepam Drugs 0.000 claims description 3
- ADIMAYPTOBDMTL-UHFFFAOYSA-N oxazepam Chemical compound C12=CC(Cl)=CC=C2NC(=O)C(O)N=C1C1=CC=CC=C1 ADIMAYPTOBDMTL-UHFFFAOYSA-N 0.000 claims description 3
- 229960000762 perphenazine Drugs 0.000 claims description 3
- RAPZEAPATHNIPO-UHFFFAOYSA-N risperidone Chemical compound FC1=CC=C2C(C3CCN(CC3)CCC=3C(=O)N4CCCCC4=NC=3C)=NOC2=C1 RAPZEAPATHNIPO-UHFFFAOYSA-N 0.000 claims description 3
- 229960001534 risperidone Drugs 0.000 claims description 3
- 229960003188 temazepam Drugs 0.000 claims description 3
- LFMYNZPAVPMEGP-PIDGMYBPSA-N Fluvoxamine maleate Chemical compound OC(=O)\C=C/C(O)=O.COCCCC\C(=N/OCCN)C1=CC=C(C(F)(F)F)C=C1 LFMYNZPAVPMEGP-PIDGMYBPSA-N 0.000 claims description 2
- GIYXAJPCNFJEHY-UHFFFAOYSA-N N-methyl-3-phenyl-3-[4-(trifluoromethyl)phenoxy]-1-propanamine hydrochloride (1:1) Chemical compound Cl.C=1C=CC=CC=1C(CCNC)OC1=CC=C(C(F)(F)F)C=C1 GIYXAJPCNFJEHY-UHFFFAOYSA-N 0.000 claims description 2
- 229960004538 alprazolam Drugs 0.000 claims description 2
- VREFGVBLTWBCJP-UHFFFAOYSA-N alprazolam Chemical compound C12=CC(Cl)=CC=C2N2C(C)=NN=C2CN=C1C1=CC=CC=C1 VREFGVBLTWBCJP-UHFFFAOYSA-N 0.000 claims description 2
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- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims 1
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 4
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- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
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- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 3
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- GDXWHFPKFUYWBE-UHFFFAOYSA-N [F].Cl Chemical compound [F].Cl GDXWHFPKFUYWBE-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 239000003463 adsorbent Substances 0.000 description 1
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- CJOFXWAVKWHTFT-XSFVSMFZSA-N fluvoxamine Chemical compound COCCCC\C(=N/OCCN)C1=CC=C(C(F)(F)F)C=C1 CJOFXWAVKWHTFT-XSFVSMFZSA-N 0.000 description 1
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- MEYZYGMYMLNUHJ-UHFFFAOYSA-N tunicamycin Natural products CC(C)CCCCCCCCCC=CC(=O)NC1C(O)C(O)C(CC(O)C2OC(C(O)C2O)N3C=CC(=O)NC3=O)OC1OC4OC(CO)C(O)C(O)C4NC(=O)C MEYZYGMYMLNUHJ-UHFFFAOYSA-N 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Sampling And Sample Adjustment (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a kind of measuring methods of smart crudefiber crop drug, utilize smart crudefiber crop drug in DGT device measurement water body, MCX resin adsorption film is made in MCX resin and agarose film with partial size between 30~40 μm, the adsorbed film is applied to based in diffusion film (DGT) technology, and selects suitable diffusion barrier, filter membrane；Suitable eluant, eluent is selected after the completion of absorption, eliminates the evaluated error of smart crudefiber crop drug to greatest extent；Present invention production raw material is cheap and easy to get, and preparation process is simple time-consuming short, is suitble to the in situ detection of smart crudefiber crop drug in water body.
Description
Technical field
The present invention relates to diffusion thin film technique fields, more specifically to a kind of measurement side of smart crudefiber crop drug
Method.
Background technique
Smart crudefiber crop drug is that one kind can directly act on central nervous system, reaches excited or inhibiting effect medicine
Product.With the quickening of modern society's life rhythm and the increase of life stress, mental disorder disease incidence is gradually risen, smart crudefiber crop
The usage amount of drug also increases with it.Currently, various water bodys of the smart crudefiber crop drug in worldwide, including sewage plant disengaging
There is detection (Wu M., et extensively in multiple water environments medium including water, surface water, underground water, seawater or even drinking water
al.,Chemosphere,2015,138,486-493).Studies have shown that nervous centralis can be directly affected by contacting smart crudefiber crop drug
System, destroy neuroendocrine, for a long time contact microly can to human health generation seriously threaten (Chad A.K., etal.,
Environ.Sci.Technol.,2006,40(23),7207-7215).Smart crudefiber crop drug also can be to the physiology of aquatic organism simultaneously
Process generation adverse effect (Chiffre, A.et al., Environ.Sci.Pollut.Res.Int., 2016,23 (6),
4964-4977).Smart crudefiber crop drug is easy to preservation in water body, is that one kind is usually widely present in water body with trace concentration
It is easy to be ignored, but with harmfulness organic pollutant.Therefore, accurate and accurate monitoring technology and method are for water ring
Analysis, research and the early warning of smart crudefiber crop drug are most important in border.And reliable, stable sampling and determination techniques not only facilitates
Assess the environmental risk of smart crudefiber crop drug, and to understand they environmental behaviour it is most important.
Currently, mainly taking the initiative sample mode to the analysis of the smart crudefiber crop drug concentration in water environment, i.e. scene is taken
Water sample simultaneously takes back experimental determination.But since smart crudefiber crop drug belongs to trace contaminant, it is therefore desirable to take a large amount of water samples, and water
Sample needs are stored refrigerated, need the preprocessing process such as to be enriched with, elute, filter by SPE pillar before sample introduction.These processes are not only
It is very cumbersome and be readily incorporated error.
Passive sampling technology is exactly that they can measure time of pollutant relative to the maximum advantage of active sampling technique
Mean concentration preferably captures the fluctuation of concentration of water pollutant, and easy to operate, time saving and energy saving, is not required to before measurement
It is smaller to introduce error for cumbersome pretreatment sample step.Diffusion thin film technique (Diffusive gradients in
Thin films, DGT) it is the one kind of the nineties in last century by Lancaster University, Britain David Williams and sky invention
Passive sampling technology based on Fick's 1st law of diffusion.Since invention, in measurement water body, available state in soils and sediments
Metal ion in terms of be widely used.But the smart crudefiber crop medicine in water body is measured using diffusion thin film technique
The research of object is not reported.
DGT device is by filter membrane, diffusion barrier and adsorbed film and fixes the plastic wrapper of this 3 tunic and forms.Wherein filter
Film is mainly used to avoid the particulate matter in environment to be measured to enter DGT device；Diffusion barrier can allow the ion free diffusing of solution state；
Adsorbed film can select different absorption materials according to experiment purpose.Therefore, a key point of DGT technical validity is measured just
It is that can it accurately quantitative determine the concentration of object and its available state in environment and (exchange in solution rapidly
Object), generally believes that influencing the factor that DGT measures target concentration and available state mainly has the absorption of adsorbed film to imitate
Fruit, dynamic exchange process in diffusion barrier of pore size and each form of diffusion barrier etc., but in practical applications still
There is the presence to aimed concn measured deviation.
Summary of the invention
1. to solve the problems, such as
For the problem that existing sampling technique is larger to crudefiber crop drug monitoring concentration error smart in water body, the present invention provides one
The measuring method of the smart crudefiber crop drug of kind.
2. technical solution
To solve the above-mentioned problems, the technical solution adopted in the present invention is as follows:
A kind of measuring method of essence crudefiber crop drug, is measured the smart crudefiber crop drug in water body to be measured using DGT technology,
It is sampled using DGT device, after sampling, adsorbed film is carried out using eluant, eluent to afford eluent, then measurement elution
The concentration of smart crudefiber crop drug in liquid；The combination film of the DGT device is MCX resin adsorption film.
Preferably, activation is distributed in agarose film using agarose film as matrix in the MCX resin adsorption film
MCX resin, the partial size of the MCX resin of the activation are 30~40 μm.
Preferably, the DGT device further includes diffusion barrier and filter membrane；The diffusion barrier is AGP test film；Described
Filter membrane is Nuclepore track etching filter membrane.
Preferably, being used in DGT technology, specific step is as follows to measure smart crudefiber crop drug in water body to be measured:
(1) assembling of DGT device: by adsorbed film, diffusion barrier and filter membrane be sequentially overlapped in DGT device pedestal and have
Between the lid of window, it is assembled into DGT device；
(2) the DGT device in step (1) placement of DGT device: is put into the suction that smart crudefiber crop drug is carried out in water body to be measured
It is attached；
(3) recycling and elution of adsorbed film: by DGT device after taking out in water body to be measured, pure water rinsing device will be adsorbed
Film removes and places in vial, obtains eluent after eluant, eluent is added；
(4) measurement of smart crudefiber crop drug: using method associated with high performance liquid chromatography-second order ms, in determination step (3)
The concentration of smart crudefiber crop drug in obtained eluent.
Preferably, specific preparation process is as follows for the adsorbed film:
(1) MCX resin is activated using methanol, and is cleaned with ultrapure water, it is spare；
(2) the MCX resin after agar powder, activation is mixed with pure water according to certain mass ratio, shakes up and is heated to boiling
Rise the agar solution for making its transparentization obtain MCX resin；
(3) the agar solution injection for the MCX resin being prepared is accompanied to two glass sheets of U-shaped Teflon material web
In gap, bubble between glass plate is squeezed out, glass plate is horizontally arranged and cools down 50~80min, solution in glass plate at room temperature
Solidification forms adsorbed film.
Preferably, in the step (1), MCX resin is activated using methanol, and specific step is as follows:
Methanol activation: in methanol solvate, being added MCX resin, impregnate, and centrifugation removes supernatant, obtains deposition solid；
The volume mass ratio of the methanol solvate and MCX resin is 7:5mL/g；
Ultrapure water cleaning: in deposition solid be added pure water concussion processing, centrifugation, remove supernatant, repeatedly for three times after, obtain
To the MCX resin of activation.
Preferably, in the step (2), the addition mass ratio of agar powder, the MCX resin of activation and pure water be 1:(8~
15):50。
Preferably, the eluant, eluent is the mixed liquor of methanol and ammonium hydroxide, and wherein ammonium hydroxide is chromatographic grade ammonium hydroxide, with mixed liquor
On the basis of, the addition volume ratio of ammonium hydroxide is 10%.
Preferably, the smart crudefiber crop drug includes antidepression class drug and/or benzodiazepines hypnotic object；Described
Antidepression class drug includes but is not limited to Fluoxetine hydrochloride FHY, Risperidone RIS, caffeine CAF, chlorpromazine hydrochloride CLO, Malaysia
One or more of sour Fluvoxamine FMA, Mirtazapine MIR, perphenazine PER, amitriptyline AMI, BUPROPIONE HCl BUP；
The benzodiazepines hypnotic object includes but is not limited to estazolam EST, diazepam DIA, Temazepam TEM, A Pu azoles
One or more of logical sequence ALP, Oxazepam OXA.
Preferably, it is characterised in that: the concentration of smart crudefiber crop drug is between 0.005~500mg/L in the water body to be measured.
3. beneficial effect
Compared with the prior art, the invention has the benefit that
(1) the present invention provides a kind of sides based on smart crudefiber crop drug in diffusion film (DGT) technology measurement water body
Method, the adsorbed film with the preparation of MCX resin are that can effectively realize the measurement of smart crudefiber crop drug in water body in conjunction with film；
(2) it the present invention provides a kind of measuring method of crudefiber crop drug smart in water body, is sampled using DGT device, chooses tool
There is the MCX resin adsorption film of high-adsorption-capacity to be assembled into DGT device with AGP test film and Nuclepore track etching filter membrane,
Reduce absorption of the filter membrane to target substance, and then eliminates because smart crudefiber crop drug monitoring caused by filter membrane suction-operated misses
Difference realizes DGT technology to the in-site detecting of crudefiber crop drug smart in water body；
(3) in water body provided by the invention smart crudefiber crop drug measuring method, the MCX resin for being 30~40 μm with partial size is
Adsorbent and agar gel, which form a film, is made MCX resin adsorption film, and production raw material is cheap and easy to get, and preparation process is simple time-consuming short；With
Agarose film is matrix, and the MCX resin (mixed type cation exchange resin) after activation, the grain of MCX resin is distributed in surface
Diameter is small, can be uniformly distributed in film matrix, compared to XAD and HLB resin adsorption film, more uniformly spreads；Meanwhile Ke Yiwei
Smart crudefiber crop drug provides more adsorption sites, and adsorption capacity is strong, has biggish adsorption capacity, tests through inventor, utilizes
The adsorption capacity of the adsorbed film of MCX resin preparation than using XAD18 resin with or the capacity of adsorbed film of HLB resin preparation respectively increase
It is 4.2 times and 3.1 times big；
(4) in water body provided by the invention smart crudefiber crop drug measuring method, in elution step after the completion of absorption, be
Highly efficient, stable elution efficiency is obtained, avoids eluent from having an impact the concentration of smart crudefiber crop drug, using methanol and ammonia
The mixed liquor of water is as eluant, eluent；Also, it is worth noting that inventor it has been investigated that methanol and ammonium hydroxide adding proportion,
Elution effect can be seriously affected, ammonium hydroxide addition is very few or does not add that elution efficiency is low, and ammonium hydroxide excessive addition elution efficiency just no longer mentions
It rises, adverse effect can be but caused to chromatographic column and mass spectrum, therefore by experimental verification discovery repeatedly, when the mass ratio of ammonium hydroxide is super
It crosses after 10%, therefore just selects 10% ratio as ammonium hydroxide in methyl alcohol.
Detailed description of the invention
Fig. 1 is the DGT apparatus structure schematic diagram for being assembled with the MCX resin adsorption film of the preparation of the embodiment of the present invention 4；
Fig. 2 is to the adsorbance of all kinds of smart crudefiber crop substances using the DGT device in the embodiment of the present invention 4 with standing time
Change, solid line is the Molded Line being calculated according to fick's first law of diffusion in figure；
Fig. 3 be using the DGT device in the embodiment of the present invention 5 at different pH to the adsorption effect of all kinds of smart crudefiber crop substances
Figure；
Fig. 4 is the suction using the DGT device in the embodiment of the present invention 6 under different ions concentration to all kinds of smart crudefiber crop substances
Attached effect picture；
Fig. 5 is the adsorption effect figure in comparative example 2 using the DGT device of different filter membranes to all kinds of smart crudefiber crop substances；
Fig. 6 is in comparative example 1 using adsorbed film made of different resins, absorption of the prepared DGT device to caffeine
Effect picture.
In figure: 1, pedestal；2, in conjunction with film；3, diffusion barrier；4, filter membrane；5, lid.
Specific embodiment
MCX resin: mixed type cation exchange resin；HLB resin: hydrophile-lipophile balance type macroporous absorbent resin；XAD18
Resin: highly polar ion exchange resin.
The present invention is further described below combined with specific embodiments below.
Embodiment 1
It is treated to be applied in DGT technology in conjunction with film using DGT technology in the present embodiment with above-mentioned MCX resin adsorption film
It surveys essence crudefiber crop drug present in water body to be measured, specific detecting step is as follows:
(1) assembling of DGT device: MCX resin adsorption film, diffusion barrier and filter membrane are sequentially overlapped in DGT pedestal and are had
Between the lid of window, it is assembled into DGT device (as shown in Figure 1), wherein the material of the pedestal of DGT device and lid is propylene
Nitrile-butadiene-styrene copolymer；
(2) placement of DGT device: the DGT device in step (1) is put into be sufficiently stirred containing smart crudefiber crop drug to be measured
Water in, place certain time.
(3) recycling and elution of resin adsorption film: by DGT device after being taken out in water body to be measured, with pure water rinsing device
Surface smut then takes out MCX resin adsorption film, is placed in vial, is added eluant, eluent (mixed liquor of methanol and ammonium hydroxide)
Eluent is obtained after ultrasonication afterwards.
(4) measurement of smart crudefiber crop drug: using method associated with high performance liquid chromatography-second order ms, in determination step (3)
The concentration of smart crudefiber crop drug in obtained eluent.
(5) calculating of smart crudefiber crop Drug absorbability amount: (I) calculates smart crudefiber crop medicine on MCX resin adsorption film according to the following formula
The adsorbance of object
M=Ce(Vg+Ve)/fe (I)
In formula, M is the adsorbance of smart crudefiber crop drug on resin adsorption film, unit ng；CeFor crudefiber crop medicine smart in eluent
The substance withdrawl syndrome of object, unit ng/mL；VgIt is the volume of resin adsorption film, unit mL；VeIt is the volume of eluent, it is single
Position is mL；feIt is the elution efficiency of smart crudefiber crop drug, is obtained by eluting the resin adsorption film of known smart crudefiber crop Drug absorbability amount
?；
According to Fick's 1st law of diffusion following formula (II) conversion DGT concentration, smart crudefiber crop substance is dense in calculating water
Degree,
CDGT=M* Δg/(D*A*t) (II)
In formula, CDGTIt is the concentration of smart crudefiber crop drug in water body, unit ng/mL；ΔgIt is the thickness of diffusion barrier and filter membrane
The sum of, unit cm；D is diffusion coefficient of the smart crudefiber crop drug in diffusion barrier, unit cm2/s；A is the window of DGT device
Area, unit cm2；T is the standing time of DGT device, unit s.
Embodiment 2
The present embodiment is substantially with embodiment 1, and difference place is only that: the adsorbed film in the present embodiment is with agarose film
The MCX resin after activation is distributed in matrix, agarose film surface, and partial size is 30~40 μm.
The preparation step of adsorbed film is as follows in the present embodiment:
(1) MCX resin is activated using methanol, and is cleaned with ultrapure water, it is spare；
(2) by after agar powder, activation MCX resin (weight in wet base) and pure water according to addition mass ratio be 1:8:50 quality
Than mixing, shakes up and heated solution to boiling makes its transparentization obtain the agar solution of MCX resin；
(3) the agar solution injection for the MCX resin being prepared is accompanied to two glass sheets of U-shaped Teflon material web
In gap, bubble between glass plate is squeezed out, glass plate is horizontally arranged and cools down 80min at room temperature, solution solidification in glass plate
Form MCX resin adsorption film.
The adsorbed film of the present embodiment can be used for smart crudefiber crop drug, be particularly suitable for the absorption inspection of antidepression class drug in water body
It surveys.Find that the antidepression class drug in water body to be measured can be one of following or a variety of exist simultaneously through detection: hydrochloric acid fluorine
Western spit of fland FHY, Risperidone RIS, caffeine CAF, chlorpromazine hydrochloride CLO, fluvoxamine maleate FMA, Mirtazapine MIR, perphenazine
PER, amitriptyline AMI, BUPROPIONE HCl BUP.
It is to be applied in DGT technology in conjunction with film with above-mentioned adsorbed film, using DGT technology on present in water body to be measured
The smart crudefiber crop drug stated is measured (detectable concentration is between 0.005~500mg/L), is sampled using DGT device, and sampling terminates
Afterwards, adsorbed film is carried out using eluant, eluent affording eluent, then measures the concentration of smart crudefiber crop drug in eluent.
Embodiment 3
Substantially with embodiment 1, difference place is only that the present embodiment:
In step (1), MCX resin is activated using methanol, and specific step is as follows:
1) methanol activates: in 70mL methanol solvate, the MCX resin of 50g is added, 30min is impregnated, then in 5000r/
Centrifugal treating 5min under the revolving speed of min removes supernatant, obtains deposition solid；
2) ultrapure water cleans: pure water concussion processing, centrifugal treating under the revolving speed of 5000r/min being added in deposition solid
5min removes supernatant, and ultrapure water cleans three times, the MCX resin activated；
3) it saves: ultrapure water is added again into the MCX resin of activation, additional amount is that liquid level is more than that MCX resin can be deposited
It puts.
Using above-mentioned steps, the activation of MCX resin may be implemented, be then distributed in agarose film, be made corresponding and inhale
Membrane.The adsorbed film of the present embodiment can be used for the absorption and analysis of benzodiazepines hypnotic object in water body, the benzene phenodiazine
Tall and erect class sleeping drug can be one of following or a variety of exist simultaneously: estazolam EST, diazepam DIA, Temazepam
TEM, alprazolam ALP, Oxazepam OXA.
Embodiment 4
For the adsorbed film of the present embodiment using agarose film as matrix, the MCX resin after activation, grain is distributed in agarose film surface
Diameter is less than 30~35 μm.
In the preparation process of this implementation adsorbed film:
In step (1), MCX resin is activated using methanol, and specific step is as follows:
1) methanol activates: in 70mL methanol solvate, the MCX resin of 50g is added, 30min is impregnated, then in 7200r/
Centrifugal treating 5min under the revolving speed of min removes supernatant, obtains deposition solid；
2) ultrapure water cleans: pure water concussion processing, centrifugal treating under the revolving speed of 7200r/min being added in deposition solid
5min removes supernatant, and ultrapure water cleans three times, the MCX resin activated；
3) it saves: ultrapure water is added again into the MCX resin of activation, additional amount is that liquid level is more than that MCX resin can be deposited
It puts, after toppling over supernatant liquor when taking, directly weighs remaining deposit (the MCX resin activated), be at this time weight in wet base state.
In step (2), agar powder, the MCX resin (weight in wet base) of activation and pure water are 1:10:50 according to addition mass ratio；
In step (3), glass plate is horizontally arranged and cools down 60min at room temperature, solution solidifies to form suction in glass plate
Membrane.
It with above-mentioned adsorbed film is to be applied in DGT technology, using DGT technology to water body to be measured in conjunction with film in the present embodiment
Present in above-mentioned smart crudefiber crop drug be measured, using the above-mentioned adsorbed film that MCX resin is distributed with being prepared as DGT
The combination film of device, diffusion barrier select AGP test film, and filter membrane selects Nuclepore track etching filter membrane.Specific detecting step
It is as follows:
(1) assembling of DGT device: by above-mentioned MCX resin adsorption film, AGP test film and the Nuclepore being prepared
Track etching filter membrane (hydrophily, diameter 25mm, 0.45 μm of aperture, whatman) is sequentially overlapped in DGT pedestal and with window
Between lid, it is assembled into DGT device (as shown in Figure 1), wherein the material of the pedestal of DGT device and lid is acrylic nitrile-butadiene two
Alkene-styrol copolymer；
(2) placement of DGT device: the DGT device in step (1) is put into be sufficiently stirred containing smart crudefiber crop drug to be measured
Water in, 3~168h of standing time, wherein the concentration of smart crudefiber crop drug is 3 μ g/L in water body to be measured.
(3) recycling and elution of resin adsorption film: by DGT device after being taken out in water body to be measured, with pure water rinsing device
Surface smut then takes out MCX resin adsorption film, is placed in vial, addition eluant, eluent (mixed liquor of methanol and ammonium hydroxide,
The two adding proportion is 9:1) eluent is obtained after ultrasonication 3h afterwards.
(4) measurement of smart crudefiber crop drug: using method associated with high performance liquid chromatography-second order ms, in determination step (3)
The concentration of smart crudefiber crop drug in obtained eluent.
(5) calculating of smart crudefiber crop Drug absorbability amount: (I) calculates smart crudefiber crop medicine on MCX resin adsorption film according to the following formula
The adsorbance of object
M=Ce(Vg+Ve)/fe (I)
In formula, M is the adsorbance of smart crudefiber crop drug on resin adsorption film, unit ng；CeFor crudefiber crop medicine smart in eluent
The substance withdrawl syndrome of object, unit ng/mL；VgIt is the volume of resin adsorption film, unit mL；VeIt is the volume of eluent, it is single
Position is mL；feIt is the elution efficiency of smart crudefiber crop drug, is obtained by eluting the resin adsorption film of known smart crudefiber crop Drug absorbability amount
?；
According to Fick's 1st law of diffusion following formula (II) conversion DGT concentration, smart crudefiber crop substance is dense in calculating water
Degree,
CDGT=M* Δg/(D*A*t) (II)
In formula, CDGTIt is the concentration of smart crudefiber crop drug in water body, unit ng/mL；ΔgIt is the thickness of diffusion barrier and filter membrane
The sum of, unit cm；D is diffusion coefficient of the smart crudefiber crop drug in diffusion barrier, unit cm2/s；A is the window of DGT device
Area, unit cm2；T is the standing time of DGT device, unit s.
In the present embodiment, wherein when measuring temperature is 25 DEG C, the diffusion system of above-mentioned measured all kinds of smart crudefiber crop substances
Number is shown in Table 1.
The diffusion coefficient of all kinds of smart crudefiber crop substances of table 1.
Window area A:2.51cm2；
It is to be determined in 3~168 hours in minute t to above-mentioned 14 kinds smart crudefiber crop drugs.
Measurement concentration (the C of above-mentioned measured all kinds of smart crudefiber crop substances is calculated according to above-mentioned formulaDGT) and actual concentrations (3
μ g/L) ratio in 0.9~1.1 range, meet DGT measurement require.As shown in Fig. 2, the essence being enriched on DGT absorption glue
The quality of crudefiber crop drug can be with DGT theoretical formula quality good agreement calculated.Illustrate the case where placing the long period
Under, DGT can measure the concentration of smart crudefiber crop drug in water well.
Embodiment 5
Substantially with embodiment 4, difference place is only that the present embodiment: is detected under different pH in the present embodiment, is utilized DGT skill
Art measures the influence of smart crudefiber crop substance in water body, wherein the concentration of smart crudefiber crop drug is 20 μ g/L in water body to be measured, it is to be measured water-soluble
The pH of liquid is respectively as follows: 3.02,5.04,6.95,8.34 and 9.42.
As shown in figure 3, the smart crudefiber crop material concentration C being calculated from the formulaDGTWith the smart crudefiber crop object in actual measurement solution
Matter concentration CsoluRatio between 0.9~1.1, illustrate that the pH of water body has not significant impact the measurement of DGT.
Embodiment 6
Substantially with embodiment 4, difference place is only that the present embodiment: the present embodiment is using essence in DGT device measurement water body
In the step of crudefiber crop drug (2), DGT assembling device is put into the water containing smart crudefiber crop drug to be measured being sufficiently stirred, when placement
Between for 24 hours, wherein the concentration of smart crudefiber crop drug is 20 μ g/L, the ion concentration (in terms of NaCl) point of aqueous solution to be measured in water body to be measured
Not are as follows: 0.1,1,10,100,500mmol/L.
As shown in figure 4, the smart crudefiber crop material concentration C being calculated from the formulaDGTWith the smart crudefiber crop object in actual measurement solution
Matter concentration CsoluRatio between 0.9~1.1, illustrate that the ionic strength of water body has not significant impact the measurement of DGT.
Comparative example 1
This comparative example is substantially with embodiment 4, and difference place is only that: there are two types of adsorbed films described in this comparative example, and one
Kind is the XAD18 resin that activation is distributed in agarose film using agarose film as matrix；Second is using agarose film as base
The HLB resin of activation is distributed in body in agarose film.
Substantially with embodiment 2, difference place is only that the preparation process of this comparative example adsorbed film:
In step (1), XAD18 resin is activated using methanol；
In step (2), the XAD18 resin after agar powder, activation is mixed with pure water according to certain mass ratio, is shaken up simultaneously
Being heated to boiling makes its transparentization obtain the agar solution of XAD18 resin；
In step (3), the agar solution injection for the XAD18 resin being prepared is accompanied into U-shaped Teflon material web
In two glass sheets gaps, bubble between glass plate is squeezed out, glass plate is horizontally arranged and is cooled down at room temperature, solution in glass plate
Solidification forms adsorbed film.
Attached test is carried out to the water body containing smart crudefiber crop drug, as shown in fig. 6, result proof is prepared into using MCX resin
To adsorbed film adsorption capacity than the absorption using XAD18 macroreticular resin and the adsorbed film being prepared using HLB resin
Capacity respectively increases 4.2 times and 3.1 times.
Comparative example 2
Firstly, it is necessary to be pointed out that filter membrane is the important component in DGT device, water body is being measured using DGT technology
In smart crudefiber crop drug when, not only need to select suitable adsorbed film, it is also necessary to select suitable filter membrane, filter membrane is for object
Adsorbance must be small as far as possible, could not influence diffusion of the object to resin adsorption film in this way, and different organic matters are in difference
Adsorption capacity on filter membrane is different, therefore must choose suitable filter membrane for target substance before method exploitation, to reduce
Its absorption or retention to detection object, causes measurement error.
This comparative example chooses four kinds of filter membranes, detects to absorption property of the smart crudefiber crop drug on filter membrane, specific steps
It is as follows:
(1) four kinds of filter membranes, respectively GH- polypropylene fibre film (GHP), Nuclepore trace-etching-film are chosen
(Nuclepore), poly (ether sulfone) film (PES) and polytetrafluoroethylene film (PTFE), by ultrapure water of the new film containing 0.01M NaCl
It impregnates one day.
(2) four kinds of films are put into 10mL to contain in the triangular flask of 20 μ g/L14 kind target essence crudefiber crop drugs, are shaken at 25 DEG C
It swings 24 hours.
(3) it is put into film front and back and takes 200 μ/L water sample from triangular flask, and survey target concentration in water sample.
(4) film is calculated to the adsorption percentage of target substance with following formula:
Adsorption%=(Ca-Cb)/Ca × 100%
Wherein CaIt is target concentration original in conical flask, CbIt is target concentration in conical flask after taking out film.
It is obtained as shown in figure 5, inventor analyzes by Specialized Theory with multiple repetition test, only Nuclepore film pair
The absorption of object is minimum, and the filter membrane of polyether sulfone or polytetrafluoroethylene (PTFE) material can largely adsorb smart crudefiber crop drug, causes the object
Matter cannot form diffusion gradient in filter membrane and diffusion barrier and be captured in turn by resin adsorption film, therefore, to essence fiber crops in water body
Filter membrane of the Nuclepore film as DGT device is chosen when substance is measured.
Comparative example 3
In addition, when carrying out trace detection using DGT technology, in addition to error caused by DGT device, to adsorbed film into
The step of row elution is equally the important source for causing measuring result error to generate.The method of the elution of methanol used at present
The smart crudefiber crop medicament elution adsorbed on MCX resin adsorption film can not be got off, therefore subsequent concentration mensuration can not be carried out.For
Highest, most stable of elution efficiency are obtained, inventor has attempted several after careful theory analysis and multiple repetition test
Different eluents, finally found that, use the mixed liquor of methanol and ammonium hydroxide as eluant, eluent, and it is best to elute effect, and pass through into
One step the study found that during elution agarose film between eluent and MCX resin contact there are certain resistances
Hinder effect, because agarose itself belongs to hydrogel, most of the inside is water, so, the adding proportion of ammonium hydroxide especially will affect
Effect is eluted, therefore this comparative example has studied influence of the additive amount of ammonium hydroxide in eluant, eluent to elution effect；Specific research step
It is as follows:
(1) eluent is prepared: preparing the methanol solution (volume respectively containing 1.0%, 1%, 5% and 10% ammonium hydroxide
Than)；
(2) step DGT assembling device the placement of DGT device: is put into 14 kinds of target essence crudefiber crop medicines that 10mL contains 20 μ g/L
It in the water of object, shakes for 24 hours, wherein the concentration of smart crudefiber crop drug is 20 μ g/L in water body to be measured；
(3) recycling and elution of resin adsorption film: concrete operations are with embodiment 1, but eluent is used respectively in step (1)
Four kinds of eluents；
(4) measurement of smart crudefiber crop drug: the concentration of smart crudefiber crop drug in eluent obtained in determination step (3)；
(5) calculating of smart crudefiber crop medicament elution efficiency: elution efficiency calculates according to the following formula
M is the quality of the smart crudefiber crop drug eluted from absorption glue, C in formulaaIt is object original in conical flask
Concentration, CbIt is target concentration in conical flask after taking out film, V is liquid volume 10mL.
The results are shown in Table 2, gradually increases the ratio of ammonium hydroxide in methanol, and elution efficiency increases.But experiment discovery,
After the mass ratio of ammonium hydroxide is more than 10%, elution efficiency is just there is no being obviously improved, and the ammonium hydroxide of overrich can be to chromatographic column
Adverse effect is caused with mass spectrum, therefore just selects 10% ratio as ammonium hydroxide in methyl alcohol.
The elution efficiency of the eluant, eluent of the different ammonium hydroxide adding proportions of table 2.
Claims (10)
1. a kind of measuring method of essence crudefiber crop drug, it is characterised in that: using DGT technology to the smart crudefiber crop drug in water body to be measured
It is measured, is sampled using DGT device, after sampling, adsorbed film is carried out using eluant, eluent to afford eluent, then
Measure the concentration of smart crudefiber crop drug in eluent；The combination film of the DGT device is MCX resin adsorption film.
2. the measuring method of essence crudefiber crop drug according to claim 1, it is characterised in that: the MCX resin adsorption film,
Using agarose film as matrix, the MCX resin of activation is distributed in agarose film, the partial size of the MCX resin of the activation is 30
~40 μm.
3. the measuring method of essence crudefiber crop drug according to claim 2, it is characterised in that: the DGT device further includes expanding
Dissipate film and filter membrane；The diffusion barrier is AGP test film；The filter membrane is Nuclepore track etching filter membrane.
4. the measuring method of smart crudefiber crop drug according to claims 1 to 3, it is characterised in that: be used in DGT technology to survey
Specific step is as follows for smart crudefiber crop drug in fixed water body to be measured:
(1) assembling of DGT device: adsorbed film, diffusion barrier and filter membrane are sequentially overlapped in the pedestal of DGT device and with window
Lid between, be assembled into DGT device；
(2) the DGT device in step (1) placement of DGT device: is put into the absorption that smart crudefiber crop drug is carried out in water body to be measured；
(3) recycling and elution of adsorbed film: by DGT device after taking out in water body to be measured, pure water rinsing device takes adsorbed film
It out and is placed in vial, obtains eluent after eluant, eluent is added；
(4) measurement of smart crudefiber crop drug: method associated with high performance liquid chromatography-second order ms is used, determination step obtains in (3)
Eluent in smart crudefiber crop drug concentration.
5. the measuring method of essence crudefiber crop drug according to claim 4, it is characterised in that: the specific preparation of the adsorbed film
Steps are as follows:
(1) MCX resin is activated using methanol, and is cleaned with ultrapure water, it is spare；
(2) the MCX resin after agar powder, activation is mixed with pure water according to certain mass ratio, shaking up and being heated to boiling makes
Its transparentization obtains the agar solution of MCX resin；
(3) the agar solution injection for the MCX resin being prepared is accompanied to two glass sheets gaps of U-shaped Teflon material web
In, bubble between glass plate is squeezed out, glass plate is horizontally arranged and cools down 50~80min at room temperature, solution solidification in glass plate
Form adsorbed film.
6. the measuring method of essence crudefiber crop drug according to claim 5, it is characterised in that: in the step (1), MCX tree
Rouge is activated using methanol, and specific step is as follows:
Methanol activation: in methanol solvate, being added MCX resin, impregnate, and centrifugation removes supernatant, obtains deposition solid；It is described
The volume mass ratio of methanol solvate and MCX resin is 7:5mL/g；
Ultrapure water cleaning: in deposition solid be added pure water concussion processing, centrifugation, remove supernatant, repeatedly for three times after, lived
The MCX resin of change.
7. the measuring method of essence crudefiber crop drug according to claim 5, it is characterised in that: in the step (2), agar powder
The addition mass ratio at end, the MCX resin of activation and pure water is 1:(8~15): 50.
8. the measuring method of smart crudefiber crop drug according to claim 5, it is characterised in that: the eluant, eluent is methanol and ammonia
The mixed liquor of water, wherein ammonium hydroxide is chromatographic grade ammonium hydroxide, and on the basis of mixed liquor, the addition volume ratio of ammonium hydroxide is 10%.
9. the measuring method of essence crudefiber crop drug according to claim 1, it is characterised in that: the smart crudefiber crop drug includes
Antidepression class drug and/or benzodiazepines hypnotic object；The antidepression class drug includes but is not limited to Fluoxetine hydrochloride
FHY, Risperidone RIS, caffeine CAF, chlorpromazine hydrochloride CLO, fluvoxamine maleate FMA, Mirtazapine MIR, perphenazine PER,
One or more of amitriptyline AMI, BUPROPIONE HCl BUP；The benzodiazepines hypnotic object includes but unlimited
In one or more of estazolam EST, diazepam DIA, Temazepam TEM, alprazolam ALP, Oxazepam OXA.
10. the measuring method of essence crudefiber crop drug according to claim 9, it is characterised in that: essence fiber crops in the water body to be measured
The concentration of class drug is between 0.005~500mg/L.
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