CN114577952B - Method for determining antiviral drug famciclovir residue in environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment - Google Patents
Method for determining antiviral drug famciclovir residue in environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment Download PDFInfo
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Abstract
The invention discloses a method for determining antiviral drug famciclovir residues in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment, which comprises the following specific processes: the method comprises the steps of extracting and enriching antiviral drug famciclovir in a sample to be detected by taking a hydrophobic eutectic solvent as an extractant of liquid-liquid microextraction, and analyzing and detecting the antiviral drug famciclovir by high performance liquid chromatography, wherein the hydrophobic eutectic solvent comprises a hydrogen bond donor and a hydrogen bond acceptor, the hydrogen bond donor is thymol or n-decanoic acid, and the hydrogen bond acceptor is ethyl aniline formate or chlorpheniramine. The invention uses self-made novel hydrophobic eutectic solvent as an extractant of a liquid-liquid microextraction technology, combines a high performance liquid chromatography technology to extract, enrich, separate and detect famciclovir in an environmental water sample, and has the advantages of simple operation, high enrichment multiple, low detection limit, good reproducibility, low cost, environmental friendliness and the like.
Description
Technical Field
The invention belongs to the technical field of extraction, separation and enrichment, and particularly relates to a method for determining antiviral drug famciclovir residues in an environmental water sample based on liquid-liquid microextraction and enrichment of a hydrophobic eutectic solvent.
Background
Antiviral drugs are a class of drugs used to prevent or treat viral infections such as influenza, hepatitis, herpes, measles, human papilloma, acquired immunodeficiency syndrome (aids), and new coronapneumonia. The seasonal influenza and influenza of human body and the pandemic diseases such as avian influenza and swine influenza of livestock need a large amount of antiviral drugs, and the seasonal changes and peak emission of antiviral drug residues are often caused. Wherein, famciclovir is a novel broad-spectrum anti-herpesvirus drug discovered in recent years, and can treat diseases such as herpes zoster, varicella, genital herpes, herpes simplex and the like. Due to its high solubility in water and easy absorption by living organisms, famciclovir has been widely used in clinical treatment. However, after famciclovir is used by humans, some of the drugs are not completely metabolized and are excreted from the body through urine or feces. In addition, pharmaceutical wastewater generated in the production process of pharmaceutical factories, and medicines which are expired or not drunk and discarded, are finally collected into sewage treatment plants through various ways. Even after treatment by sewage treatment plants, a significant portion of these drugs are more difficult to remove or degrade and thus enter the surrounding waters and remain for a long period of time. Because of the high biological activity, the medicines can generate drug-resistant virus strains in certain organisms, and greatly weaken the therapeutic effect of antiviral medicines on human bodies and animals. Adverse effects of antiviral drugs and their metabolites on aquatic organisms and ecosystems have attracted widespread public health attention. Therefore, the establishment of a simple, accurate and efficient enrichment and determination method is necessary for grasping the residual level of famciclovir antiviral drugs in environmental water.
Methods reported in the literature to date for analysis of antiviral drug residues include spectrophotometry, liquid chromatography-tandem mass spectrometry (LC-MS/MS), ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), gas chromatography-tandem mass spectrometry, and fluorescence. However, these assays are primarily directed to the determination of antiviral drug residues in tablets and biological matrices. So far, few studies have been conducted to determine antiviral drug residues in environmental water samples. The method is mainly characterized in that the antiviral drug has strong hydrophilicity, the matrix components of the water sample are complex, and the residual concentration of the antiviral drug in the water is low (ng/L-mg/L level), so that the determination difficulty of the antiviral drug in the water sample is increased. Thus, the necessary enrichment pretreatment of the water sample is required before its concentration of famciclovir Wei Canliu is determined. And most of organic solvents used in the conventional sample pretreatment process have strong volatility and high toxicity, and are easy to cause harm to human bodies and the environment. Therefore, there is an urgent need to find a green extractant which is low in toxicity, non-volatile, good in extraction performance, strong in hydrophobicity and low in cost, as a substitute.
The hydrophobic eutectic solvent is a novel green extractant which rapidly rises in recent years, and has the excellent characteristics of low toxicity, high chemical stability, good thermal stability, low vapor pressure and the like similar to ionic liquids. In addition, the method has the unique advantages of simple preparation process, low price, 100% of atom utilization rate, easiness in biodegradation and the like, and can effectively enrich and separate target analytes in the water phase.
The invention establishes a novel method for determining antiviral drug famciclovir residues in an environmental water sample by combining a liquid-liquid microextraction technology based on a hydrophobic eutectic solvent and a high performance liquid chromatography technology.
Disclosure of Invention
The invention solves the technical problem of providing a novel method for measuring the antiviral drug famciclovir residue in an environmental water sample by using a liquid-liquid microextraction technology based on a hydrophobic eutectic solvent, which has the advantages of low cost, simple operation, high sensitivity and environmental friendliness.
The invention adopts the following technical scheme to solve the technical problems, and is characterized in that the method for determining antiviral drug famciclovir residues in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment comprises the following specific processes: the method comprises the steps of extracting and enriching antiviral drug famciclovir in a sample to be detected by taking a hydrophobic eutectic solvent as an extracting agent for liquid-liquid microextraction, and analyzing and detecting the antiviral drug famciclovir by high performance liquid chromatography, wherein the hydrophobic eutectic solvent comprises a hydrogen bond donor and a hydrogen bond acceptor, the hydrogen bond donor is thymol or n-decanoic acid, the hydrogen bond acceptor is ethyl aniline formate or chlorpheniramine, and the molar ratio of the hydrogen bond acceptor to the hydrogen bond donor is 10:1-1:10.
Further defined, the density of the hydrophobic eutectic solvent ranges from 0.9419 g/cm to 1.1255g/cm 3 The viscosity is 24-255 mPa.s, the contact angle is 43.5-67.0 DEG, and the melting point is-57.3-38.4 ℃.
Further defined, the specific preparation process of the hydrophobic eutectic solvent comprises the following steps: and placing the hydrogen bond donor and the hydrogen bond acceptor in a reaction container, heating and stirring at 40-100 ℃ for 5-60 min to obtain a clear and transparent solution, namely the hydrophobic eutectic solvent.
Further defined, the method for determining antiviral drug famciclovir residues in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment is characterized by comprising the following specific steps:
step S1: respectively adding 50mg of hydrophobic eutectic solvent into a 10mL glass centrifuge tube filled with 5mL of famciclovir Wei Biaozhun solution with different gradient concentrations, performing vortex dispersion for 1.5min to uniformly mix the hydrophobic eutectic solvent and the famciclovir Wei Biaozhun solution, centrifuging at 2500rpm/min for 5min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase, discarding the water phase, reserving the hydrophobic eutectic solvent phase, adding 200 mu L of methanol to dilute the hydrophobic eutectic solvent phase, taking 20 mu L of methanol to inject the solution into a high performance liquid chromatograph for analysis, measuring the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and drawing a standard curve of famciclovir concentration corresponding to the peak area of a chromatogram;
step S2: and transferring 5mL of the pretreated sample to be detected into a 10mL glass centrifuge tube, adding 50mg of hydrophobic eutectic solvent, performing vortex dispersion for 1.5min to uniformly mix the hydrophobic eutectic solvent and the sample solution to be detected, centrifuging at 2500rpm/min for 5min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase, discarding the water phase, reserving the hydrophobic eutectic solvent phase, adding 200 mu L of methanol to dilute the hydrophobic eutectic solvent phase, taking 20 mu L of methanol to inject the 20 mu L of methanol into a high performance liquid chromatograph for analysis, determining the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and performing quantitative detection on famciclovir in the sample to be detected according to the peak area of a chromatogram of the sample to be detected and combining a standard curve of the peak area of the chromatogram in combination with the famciclovir concentration.
Further limiting, the sample to be detected is an environmental water sample, wherein the environmental water sample comprises one or more of tap water, mineral water, purified water, snow water, river water, lake water or effluent of a sewage plant, and the environmental water sample is filtered by a water phase microporous filter membrane of 0.45 mu m and 0.22 mu m for later use before analysis.
Further limited, the chromatographic column adopted by the high performance liquid chromatograph in the high performance liquid chromatography is a Wondasil C18 liquid chromatographic column, the specification is 250mm multiplied by 4.6mm, the particle size is 5 μm, the chromatographic column temperature is 30 ℃, the sample injection volume is 20 μl, the detector wavelength is 305nm, the mobile phase A is chromatographic methanol, the mobile phase B is ultrapure water, the flow rate is 0.6mL/min, and the elution mode is: 0-5 min, 70-80% (A); 5-6 min, 80-90% (A); 6-7 min, 90-100% (A); 7-12 min,100% (A); 12-13 min, 100-70% (A).
Compared with the prior art, the invention has the following advantages and beneficial effects: the hydrophobic eutectic solvent has remarkable enrichment effect on the famciclovir Wei Cuiqu in an environmental water sample. Compared with the prior art, the invention uses the self-made novel hydrophobic eutectic solvent as the extractant of the liquid-liquid microextraction technology, combines the high performance liquid chromatography technology to extract, enrich, separate and detect the famciclovir in the environmental water sample, and has the advantages of simple operation, high enrichment factor, low detection limit, good reproducibility, low cost, environmental friendliness and the like.
Detailed Description
The above-described matters of the present invention will be described in further detail by way of examples, but it should not be construed that the scope of the above-described subject matter of the present invention is limited to the following examples, and all techniques realized based on the above-described matters of the present invention are within the scope of the present invention.
Example 1
Taking a certain amount of thymol and ethyl aniline formate according to the molar ratio of (1:1, 1:2, 1:3, 2:1 and 3:1), placing the mixture into a round bottom flask, and stirring for 0.5h under the heating condition of 45 ℃ until a clear transparent liquid, namely a hydrophobic eutectic solvent, is formed, wherein the clear transparent liquid is in the range of 25-100 ℃.
Example 2
Taking a certain amount of thymol and chlorpheniramine according to the molar ratio of (1:1, 1:2, 1:3, 2:1 and 3:1), respectively, placing the mixture into a round bottom flask, and stirring for 0.5h under the heating condition of 45 ℃ until a clear transparent liquid, namely a hydrophobic eutectic solvent, is formed, wherein the clear transparent liquid is in the range of 25-100 ℃.
Example 3
Taking a certain amount of n-decanoic acid and ethyl aniline formate according to the molar ratio of (1:1, 1:2, 1:3, 2:1 and 3:1), placing the mixture into a round-bottom flask, and stirring for 0.5h under the heating condition of 45 ℃ until a clear transparent liquid, namely a hydrophobic eutectic solvent, is formed, wherein the clear transparent liquid is in the range of 25-100 ℃.
Example 4
Taking a certain amount of n-decanoic acid and chlorpropham respectively according to the molar ratio of (1:1, 1:2, 1:3, 2:1 and 3:1), then placing the mixture into a round bottom flask, and stirring for 0.5h under the heating condition of 45 ℃ until a clear transparent liquid, namely a hydrophobic eutectic solvent, is formed, wherein the clear transparent liquid is in the range of 25-100 ℃.
Example 5
Determination of famciclovir in actual environmental water sample
(1) Experimental facilities: a Waters high performance liquid chromatograph equipped with a 1525 pump, a model 1500 column oven and a 2998 photodiode array detector; wondasil C18 liquid chromatography column (4.6X1250 mm, particle size 5 μm), column temperature 30 ℃, sample volume 20. Mu.L, detector wavelength 305nm. Mobile phase A was chromatographic methanol, mobile phase B was ultrapure water, and the flow rate was 0.6mL/min. The elution mode is: 0-5 min, 70-80% (A); 5-6 min, 80-90% (A); 6-7 min, 90-100% (A); 7-12 min,100% (A); 12-13 min, 100-70% (A).
(2) Pretreatment of actual samples: the sample to be measured is an actual environmental water sample, the environmental water sample comprises one or more of tap water, mineral water, purified water, snow water, river water, lake water or water outlet water of a sewage plant, and the environmental water sample is filtered by a water phase microporous filter membrane with the diameter of 0.45 mu m and 0.22 mu m for standby before analysis and detection.
(3) Evaluation of measurement method: 5mL of prepared famciclovir Wei Biaozhun solution with different gradient concentrations are respectively placed in a 10mL centrifuge tube, 50mg of self-made hydrophobic eutectic solvent (thymol is taken as a hydrogen bond donor, ethyl aniline is taken as a hydrogen bond acceptor, the molar ratio is 3:1) is added, vortex dispersion is carried out for 1.5min to ensure that the two solutions are uniformly mixed, and then centrifugation is carried out for 5min at the rotating speed of 2500rpm/min to obtain obviously separated two-phase liquid, namely water phase and hydrophobic eutectic solvent phase. The aqueous phase was then discarded, the hydrophobic eutectic solvent phase (containing famciclovir) was retained in the centrifuge tube, and 200 μl of methanol was then added to allow for the followingThe method is compatible with chromatographic mobile phase, 20 mu L of the solution is injected into a high performance liquid chromatograph for analysis, the peak area response value of famciclovir in the hydrophobic eutectic solvent phase is measured, and a standard curve of the famciclovir concentration corresponding to the peak area is drawn, wherein each experiment is performed in parallel for 3 times. The obtained linear regression equation and the correlation coefficient are shown in Table 1, and as can be seen from Table 1, the obtained standard curve has a good linear relationship, and the correlation coefficient (R 2 ) The detection limit (LOD, S/N=3) was 0.9997, and the quantitative limit (LOQ, S/N=10) was 2. Mu.g/L.
Table 1 method analysis of performance
(4) Actual sample measurement: placing 5mL of the pretreated environmental water sample to be tested into a 10mL centrifuge tube, adding 50mg of synthesized hydrophobic eutectic solvent (thymol is taken as a hydrogen bond donor, ethyl aniline is taken as a hydrogen bond acceptor, the molar ratio is 3:1), carrying out vortex dispersion for 1.5min to uniformly mix the two, and centrifuging for 5min at a rotating speed of 2500rpm/min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase. And then discarding the water phase, reserving the hydrophobic eutectic solvent phase (containing famciclovir) in a centrifuge tube, adding 200 mu L of methanol to be compatible with the chromatographic mobile phase, taking 20 mu L of methanol to be injected into a high performance liquid chromatograph for analysis, determining the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and comparing with a standard curve of the peak area corresponding to the famciclovir concentration to finish the quantitative detection of famciclovir.
(5) Actual sample labeling recovery rate measurement: taking 5mL of actual environment water sample with the concentration of 50 mug/L, 500 mug/L and 1000 mug/L of famciclovir respectively into a 10mL centrifuge tube, adding 50mg of self-made hydrophobic eutectic solvent (thymol is taken as a hydrogen bond donor, ethyl aniline formate is taken as a hydrogen bond acceptor, and the molar ratio is 3:1), carrying out vortex dispersion for 1.5min to uniformly mix the hydrophobic eutectic solvent and the famciclovir solution, and centrifuging for 5min at a rotating speed of 2500rpm/min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase. And then discarding the water phase, reserving the hydrophobic eutectic solvent phase (containing famciclovir), adding 200 mu L of methanol to be compatible with the chromatographic mobile phase, taking 20 mu L of methanol to be injected into a high performance liquid chromatograph for analysis, determining the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and comparing with the standard concentration response value to complete the measurement of the recovery rate of the standard sample famciclovir. The extraction recovery rate after the method is added with the standard is 80% -120%, and the Relative Standard Deviation (RSD) is less than 10%.
While the basic principles, principal features and advantages of the present invention have been described in the foregoing examples, it will be appreciated by those skilled in the art that the present invention is not limited by the foregoing examples, but is merely illustrative of the principles of the invention, and various changes and modifications can be made without departing from the scope of the invention, which is defined by the appended claims.
Claims (5)
1. The method for determining the antiviral drug famciclovir residue in the environmental water sample based on the hydrophobic eutectic solvent liquid-liquid microextraction enrichment is characterized by comprising the following specific steps: the method comprises the steps of extracting and enriching antiviral drug famciclovir in a sample to be detected by taking a hydrophobic eutectic solvent as an extractant of liquid-liquid microextraction, and analyzing and detecting the antiviral drug famciclovir by high performance liquid chromatography, wherein the hydrophobic eutectic solvent comprises a hydrogen bond donor and a hydrogen bond acceptor, the hydrogen bond donor is thymol, the hydrogen bond acceptor is ethyl aniline formate, and the molar ratio of the hydrogen bond donor to the hydrogen bond acceptor is 3:1.
2. The method for determining antiviral drug famciclovir residue in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment according to claim 1, wherein the specific preparation process of the hydrophobic eutectic solvent is as follows: and placing the hydrogen bond donor and the hydrogen bond acceptor in a reaction container, heating and stirring at 40-100 ℃ for 5-60 min to obtain a clear and transparent solution, namely the hydrophobic eutectic solvent.
3. The method for determining antiviral drug famciclovir residue in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment according to claim 1, which is characterized by comprising the following specific steps:
step S1: respectively adding 50mg of hydrophobic eutectic solvent into a 10mL glass centrifuge tube filled with 5mL of famciclovir Wei Biaozhun solution with different gradient concentrations, performing vortex dispersion for 1.5min to uniformly mix the hydrophobic eutectic solvent and the famciclovir Wei Biaozhun solution, centrifuging at 2500rpm/min for 5min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase, discarding the water phase, retaining the hydrophobic eutectic solvent phase, adding 200 mu L of methanol to be compatible with chromatographic mobile phase, taking 20 mu L of methanol to be injected into a high performance liquid chromatograph for analysis, measuring the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and drawing a standard curve of famciclovir concentration corresponding to the peak area of a chromatogram;
step S2: and transferring 5mL of the pretreated sample to be detected into a 10mL glass centrifuge tube, adding 50mg of hydrophobic eutectic solvent, performing vortex dispersion for 1.5min to uniformly mix the hydrophobic eutectic solvent and the sample solution to be detected, centrifuging at 2500rpm/min for 5min to obtain obviously separated two-phase liquid, namely a water phase and a hydrophobic eutectic solvent phase, discarding the water phase, reserving the hydrophobic eutectic solvent phase, adding 200 mu L of methanol to be compatible with a chromatographic mobile phase, taking 20 mu L of methanol to be injected into a high performance liquid chromatograph for analysis, determining the peak area response value of famciclovir in the hydrophobic eutectic solvent phase, and performing quantitative detection on the famciclovir in the sample to be detected according to the peak area of the chromatogram of the sample to be detected and combining a standard curve of the famciclovir concentration corresponding to the peak area of the chromatogram.
4. The method for determining antiviral drug famciclovir residue in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment according to claim 1, wherein the method is characterized by: the sample to be measured is an environmental water sample, the environmental water sample comprises one or more of tap water, mineral water, purified water, snow water, river water, lake water or effluent of a sewage plant, and the environmental water sample is filtered by a water phase microporous filter membrane of 0.45 mu m and 0.22 mu m for later use before analysis.
5. The method for determining antiviral drug famciclovir residue in an environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment according to claim 1, wherein the method is characterized by: the chromatographic column adopted by the high performance liquid chromatograph in the high performance liquid chromatography is a WondaSil C18 liquid chromatographic column, the specification of the chromatographic column is 250mm multiplied by 4.6mm, the particle size is 5 mu m, the temperature of the chromatographic column is 30 ℃, the sample injection volume is 20 mu L, the wavelength of a detector is 305nm, the mobile phase A is chromatographic methanol, the mobile phase B is ultrapure water, the flow rate is 0.6mL/min, and the elution mode is as follows: 0-5 min, 70-80% of A; 5-6 min, 80-90% of A; 6-7 min,90% -100% of A; 7-12 min,100% A; 12-13 min,100% -70% of A.
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| 疏水性低共熔溶剂对水中5种非甾体抗炎药物的萃取研究;张华;陈强;刘永静;;药学研究(第06期);全文 * |
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