CN112198262A - Method for detecting non-steroidal anti-inflammatory drugs in water sample - Google Patents
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Abstract
The invention provides a method for detecting non-steroidal anti-inflammatory drugs in a water sample, and belongs to the technical field of water quality monitoring. Firstly, non-steroidal anti-inflammatory drugs in a water sample are enriched by dispersive micro-solid phase extraction, then the non-steroidal anti-inflammatory drugs are further enriched by homogeneous liquid-liquid micro-extraction, and finally the content of the non-steroidal anti-inflammatory drugs is determined by high performance liquid chromatography. The sensitivity and selectivity of the detection of the non-steroidal anti-inflammatory drugs are improved by the combination of dispersive micro-solid phase extraction, homogeneous phase liquid-liquid micro-extraction and high performance liquid chromatography, the pretreatment time of the analysis and detection is greatly shortened to about 5min, and the analysis and detection efficiency of the non-steroidal anti-inflammatory drugs in the water sample is improved. In addition, only a certain amount of SHS solution is used in the analysis and detection process to replace the traditional organic solvent, so that the method is green and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of water quality monitoring, and particularly relates to a method for detecting non-steroidal anti-inflammatory drugs in a water sample.
Background
Non-steroidal anti-inflammatory drugs (NSAIDs) have the effects of resisting inflammation, rheumatism, pain relief, fever abatement, anticoagulation and the like, are widely used for relieving osteoarthritis, rheumatism, rheumatoid arthritis, various fever and various pain symptoms clinically, about 3000 million people use the drugs every day around the world, and along with the increase of the use of the NSAIDs, the adverse reactions of the drugs are also more and more concerned by people, such as adverse reactions of gastrointestinal discomfort, liver and kidney injury, allergy and the like. A large number of NSAIDs eventually enter the water environment and become one of the new important pollutants in the water environment, and NSAIDs at different concentration levels have been detected in rivers of many countries.
In the prior art, the detection technology of NSAIDs in a water sample comprises liquid phase extraction, solid phase extraction, dispersion liquid-liquid microextraction, stirring rod adsorption extraction and the like, and the methods not only need to use a large amount of organic solvents and easily cause secondary pollution to the environment, but also have low detection sensitivity and often cannot meet the requirements of analysis and determination. Therefore, it is necessary to establish a sensitive, rapid and green detection method for detecting and analyzing the residual NSAIDs in the water sample.
Disclosure of Invention
In view of the above, the present invention provides a method for detecting a non-steroidal anti-inflammatory drug in a water sample, so as to solve the technical problems of low detection sensitivity, low detection efficiency and easy secondary pollution in the prior art during the detection of the non-steroidal anti-inflammatory drug in the water sample.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a method for detecting non-steroidal anti-inflammatory drugs in a water sample comprises the following steps:
dispersed micro solid phase extraction: adding the solid-phase extraction material into a water sample containing NSAIDs, and performing magnetic separation after full dispersion to obtain an extraction product;
acid hydrolysis: adding an acidic solution into the extraction product to dissolve the solid-phase extraction product to obtain a solution A;
homogeneous liquid-liquid microextraction: adding an SHS solution into the solution A to perform homogeneous liquid-liquid microextraction to obtain an extract B;
layering: adding an alkaline solution into the extract B, and inducing layering to obtain a supernatant C;
high performance liquid chromatography determination: and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
Specifically, the method comprises the following steps:
taking 5ml of water sample containing NSAIDs, and adjusting the pH value of the water sample to 5-10;
adding 5-30 mg of solid phase extraction material, carrying out vortex dispersion for 3-20 min, and carrying out magnetic separation to obtain a solid phase extraction product;
adding 100-800 mul of 2-6 mol/L acid solution, and dissolving the solid phase extraction product to obtain solution A;
adding 100-800 microliter SHS solution into the solution A, and performing homogeneous extraction to obtain extract B;
adding 100-400 mu L of alkaline solution with the concentration of 2-6 mol/L into the extract B, and inducing layering to obtain supernatant C;
and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
Preferably, the solid-phase extraction material is magnetic layered double hydroxide Fe3O4@ZnAl-LDH。
Preferably, the acidic solution is one of sulfuric acid, hydrochloric acid, nitric acid and trifluoroacetic acid.
Preferably, the SHS solution is one of dipropylamine, triethylamine and N, N-dimethylcyclohexylamine.
Preferably, the alkaline solution is sodium hydroxide or potassium hydroxide.
Preferably, in the step of determining the content of NSAIDs in the supernatant C by high performance liquid chromatography, the chromatographic conditions are as follows:
the chromatographic column is an Agilent ZORBAX-C18 column (250mm × 4.6mm I.D.,5 μm); protection of the column: easy guard C18 guard column (8mm x 4mm i.d.,5 μm); the mobile phase is acetonitrile-0.1% hexanoic acid water solution (68:32, v/v) with flow rate of 1.0mL min-1The detection wavelength is 254nm, and the column temperature is 25 ℃.
Preferably, the non-steroidal anti-inflammatory drug comprises one or more of ketoprofen, naproxen, and tolmetin.
According to the technical scheme, the invention provides a method for detecting non-steroidal anti-inflammatory drugs in a water sample, which has the following beneficial effects: firstly, enriching the non-steroidal anti-inflammatory drugs in a water sample by dispersive micro-solid phase extraction, then further enriching the non-steroidal anti-inflammatory drugs by adopting a homogeneous liquid-liquid micro-extraction method, and finally determining the content of the non-steroidal anti-inflammatory drugs by utilizing high performance liquid chromatography. The sensitivity and selectivity of the detection of the non-steroidal anti-inflammatory drugs are improved by the combination of dispersive micro-solid phase extraction, homogeneous phase liquid-liquid micro-extraction and high performance liquid chromatography, the pretreatment time of the analysis and detection is greatly shortened to about 5min, and the analysis and detection efficiency of the non-steroidal anti-inflammatory drugs in the water sample is improved. In addition, only a certain amount of SHS solution is used in the analysis and detection process to replace the traditional organic solvent, so that the method is green and environment-friendly.
Drawings
Figure 1 is a schematic diagram of the structure of LDH.
FIG. 2 is Fe3O4(a)、Fe3O4FT-IR spectrum of @ ZnAl-LDH (b).
FIG. 3 is Fe3O4The XRD pattern of @ ZnAl-LDH.
FIG. 4 is Fe3O4A hysteresis loop of @ ZnAl-LDH.
FIG. 5 is Fe3O4@ ZnAl-LDH nitrogen adsorption-desorption isotherm.
FIG. 6 is a chromatogram of a standard mixed solution (1.0. mu.g/mL) and a simulated water sample (5ng/mL), where 1,2,3 are TLM, KEP and NAP, respectively.
Detailed Description
The technical scheme and the technical effect of the invention are further elaborated in the following by combining the drawings of the invention.
In one embodiment, a method for detecting a non-steroidal anti-inflammatory drug in a water sample comprises the following steps:
dispersed micro solid phase extraction: and adding the solid-phase extraction material into a water sample containing the NSAIDs, and performing magnetic separation after full dispersion to obtain an extraction product.
Wherein the solid phase extraction material is magnetic layered double hydroxide Fe3O4With reference to fig. 1, a Layered Double Hydroxide (LDH), also called hydrotalcite-like, has a Layered crystal structure composed of two or more metal elements. The surface of the LDH sheets contain cations, and anions intercalated between the layers balance these cations so that the overall material is electrically neutral.
Anions between LDH layers are combined with metal ions on the surface of the layer mainly through electrostatic acting force, and the acting force is weak, so that the anions between the layers are easily replaced by other anions. In general, the more the charge and the smaller the radius of the anion, the stronger the exchange capacity, and this good interlayer anion displacement property allows LDHs to exhibit great potential in the extraction of anionic compounds.
Magnetic layered double hydroxide Fe3O4The @ ZnAl-LDH can be prepared by coprecipitation method, taking Fe3O4Placing the particles in distilled water, and performing ultrasonic dispersion to obtain Fe3O4Suspending the solution; weighing NaOH and Na2CO3Placing in a beaker, adding water to obtain mixed alkaline solution, and weighing Zn (NO)3)2·6H2O and Al (NO)3)3·9H2Placing O in a beaker, adding distilled water for ultrasonic dissolution to prepare a mixed salt solution, and gradually dropwise adding the mixed salt solution to the Fe3O4Dispersing the solution, continuously dripping mixed alkali liquor to maintain the pH value of the reaction system, and magnetically separating the synthesized Fe after complete titration3O4@ ZnAl-LDH, and washing and drying.
For example, in the above process, Fe is taken3O4Placing the particles in distilled water, and performing ultrasonic dispersion to obtain Fe3O4And (4) suspending the solution. Weighing NaOH and Na2CO3Placing in a container, adding water to obtain mixed alkaline solution, preferably NaOH and Na2CO3The molar ratio of (1) to (3). Separately weighing Zn (NO)3)2·6H2O and Al (NO)3)3·9H2And placing the mixture into a container, adding distilled water for ultrasonic dissolution, and preparing a mixed salt solution. Preferably, Zn (NO)3)2·6H2O and Al (NO)3)3·9H2The molar ratio of O is 1 (1-4). Gradually dropwise adding the mixed salt solution to the Fe3O4Dispersing the solution, and continuously dropping the mixed alkali solution to maintain the pH value of the reaction system, for example, controlling the pH value of the reaction system to be 9.5-11.0. After titration is complete, the Fe synthesized is separated magnetically3O4And washing and drying the @ ZnAl-LDH. Preferably, the synthesized Fe is sequentially treated by using 95 percent ethanol and distilled water3O4Washing with @ ZnAl-LDH, and drying at 50-100 deg.C for 6-12 hr.
In one embodiment, Fe3O4Preparation of @ ZnAl-LDH, 11.56g (0.05mol) of Fe3O4Placing the particles in distilled water, and performing ultrasonic dispersion to obtain Fe3O4And (4) suspending the solution. 4g (0.1mol) of NaOH and 10.6g (0.1mol) of Na were weighed out2CO3Placing in a beaker, and adding water to prepare mixed alkali liquor. 14.54g (0.05mol) Zn (NO) was weighed in3)2·6H2O and 18.76g (0.05mol) Al (NO)3)3·9H2And placing the mixture into a container, adding distilled water for ultrasonic dissolution, and preparing a mixed salt solution. Gradually dropwise adding the mixed salt solution to the Fe3O4Dispersing the solution while continuously dropping the mixed alkali liquor to maintain the pH value of the reaction system at 11. After titration is complete, the Fe synthesized is separated magnetically3O4@ ZnAl-LDH, sequential reaction of synthesized Fe with 95% ethanol and distilled water3O4@ ZnAl-LDH, and drying at a drying temperature of 50 ℃ for 12 h.
In yet another embodiment, Fe3O4Preparation of @ ZnAl-LDH, in one example, Fe3O4Preparation of @ ZnAl-LDH from 6.93g (0.03mol) of Fe3O4Placing the particles in distilled water, and performing ultrasonic dispersion to obtain Fe3O4And (4) suspending the solution. 4g (0.1mol) of NaOH and 31.8g (0.3mol) of Na were weighed out2CO3Placing in a beaker, and adding water to prepare mixed alkali liquor. 2.91g (0.01mol) Zn (NO) was weighed out separately3)2·6H2O and 15g (0.04mol) Al (NO)3)3·9H2And placing the mixture into a container, adding distilled water for ultrasonic dissolution, and preparing a mixed salt solution. Gradually dropwise adding the mixed salt solution to the Fe3O4Dispersing the solution, and continuously dropwise adding the mixed alkali liquor to maintain the pH value of the reaction system to be 9.5. After titration is complete, the Fe synthesized is separated magnetically3O4@ ZnAl-LDH, sequential reaction of synthesized Fe with 95% ethanol and distilled water3O4@ ZnAl-LDH, and drying at 100 deg.C for 6 h.
In yet another embodiment, Fe3O4Preparation of @ ZnAl-LDH from 6.93g (0.03mol) of Fe3O4Placing the particles in distilled water, and performing ultrasonic dispersion to obtain Fe3O4And (4) suspending the solution. 4g (0.1mol) of NaOH and 21.2g (0.2mol) of Na were weighed out2CO3Placing in a beaker, and adding water to prepare mixed alkali liquor. Separately, 5.82g (0.02mol) of Zn (NO) was weighed3)2·6H2O and 7.5g (0.02mol) Al (NO)3)3·9H2And placing the mixture into a container, adding distilled water for ultrasonic dissolution, and preparing a mixed salt solution. Gradually dropwise adding the mixed salt solution to the Fe3O4Dispersing the solution, and continuously dropwise adding the mixed alkali liquor to maintain the pH value of the reaction system to be 10. After titration is complete, the Fe synthesized is separated magnetically3O4@ ZnAl-LDH, sequential reaction of synthesized Fe with 95% ethanol and distilled water3O4@ ZnAl-LDH, and drying at a drying temperature of 70 ℃ for 6 h.
As shown in FIG. 2, Fe is given separately3O4(a)、Fe3O4FT-IR spectrum of @ ZnAl-LDH (b), in spectrum (a), 594cm-1A broader characteristic absorption peak of Fe-O was observed, indicating the presence of magnetic particles; in the map (b), 3453cm-1The absorption peaks are the expansion vibration peaks of O-H and interlayer water molecules on the laminate; 1630cm-1The absorption peaks appearing left and right are attributed to bending vibration of interlayer water molecules; 1365cm-1The absorption peaks at the left and right may be caused by CO3 2-Is caused by symmetric stretching vibration, the synthesized material is CO3 2-Intercalated LDH, while comparing pattern (a) with Fe in pattern (b)3O4The intensity of the characteristic absorption peak of (A) is significantly reduced, indicating a core-shell structure (Fe)3O4@ ZnAl-LDH).
Fe3O4The XRD pattern of @ ZnAl-LDH is shown in figure 3, Fe3O4The XRD pattern of the compound shows characteristic diffraction peaks at 18.2 degrees, 30.1 degrees, 35.4 degrees, 43.1 degrees, 57.0 degrees and 62.5 degrees; in Fe3O4Water-like of @ ZnAl-LDH is observed at 11.6 °,23.4 °,34.5 °,39.1 °,46.6 °,60.1 ° and 61.4 ° 2 θ in the XRD pattern of @ ZnAl-LDHDiffraction peaks of the characteristic crystal planes of talc, and Fe3O4Disappearance or decrease of diffraction peak of (A), indicating Fe3O4The surface is successfully coated with LDH materials.
Fe at room temperature3O4The hysteresis loop of @ ZnAl-LDH is shown in FIG. 4, and it is understood from the graph that Fe was synthesized3O4The coercive force of @ ZnAl-LDH is 0, indicating that Fe3O4@ ZnAl-LDH has good paramagnetism. Fe3O4And Fe3O4The saturation magnetic strengths of @ ZnAl-LDH were 77.8emu/g and 23.6emu/g, respectively.
Fe3O4The nitrogen adsorption-desorption isotherm of @ ZnAl-LDH is shown in FIG. 5, and it is understood from the graph that Fe was synthesized3O4The nitrogen adsorption and desorption line of @ ZnAl-LDH is a type II isothermal line and belongs to a typical non-hole type structure.
Please refer to Table 1, Fe3O4Specific surface area S of @ ZnAl-LDHBETIs 47.3m2G, pore volume VtIs 0.2042cm3In g, average pore diameter of
TABLE 1 Fe3O4Comparison of specific surface area, pore volume and pore diameter of @ ZnAl-LDH
S200, acid hydrolysis: and adding an acidic solution into the solid-phase extraction product to dissolve the solid-phase extraction product to obtain a solution A.
Specifically, an acidic solution is added to the solid-phase extraction product obtained in step S100, and the magnetic layered double hydroxide Fe is added3O4And the @ ZnAl-LDH and the non-steroidal anti-inflammatory drug adsorbed on the @ ZnAl-LDH are dissolved to form a solution A. Wherein the acid solution is one of sulfuric acid, hydrochloric acid, nitric acid and trifluoroacetic acid, and the concentration of the acid solution is 2-6 mol/L.
S300, homogeneous phase liquid-liquid microextraction: adding SHS solution into the solution A for homogeneous extraction to obtain extract B.
Wherein the SHS solution is one of dipropylamine, triethylamine and N, N-dimethylcyclohexylamine. A switching polar solvent (SHS) is a liquid that can be switched between different polarities, usually by adjusting the pH of the solution. Tertiary and secondary amines are often used in SHS, where the hydrophobic tertiary/secondary amine is converted to a hydrophilic amine salt under acidic conditions, and the original hydrophobicity is restored by the addition of an alkaline solution. As a novel extraction solvent, SHS is widely applied to the field of extraction in recent years, and compared with the traditional organic extraction solvent, SHS has unique advantages, such as simple preparation, extraction and separation, no toxicity, stability, low price, environmental protection and the like. The SHS is applied to the field of micro-extraction, so that the use of toxic extraction solvent can be avoided, the environmental pollution is reduced, and the health of experiment operators is guaranteed.
S400, layering: and adding an alkaline solution into the extract B, and inducing layering to obtain a supernatant C.
Wherein the alkaline solution is sodium hydroxide or potassium hydroxide, and the concentration is 2-6 mol/L.
High performance liquid chromatography determination: and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
Specifically, the chromatographic conditions were:
the chromatographic column is an Agilent ZORBAX-C18 column (250mm × 4.6mm I.D.,5 μm); protection of the column: easy guard C18 guard column (8mm x 4mm i.d.,5 μm); the mobile phase is acetonitrile-0.1% hexanoic acid water solution (68:32, v/v) with flow rate of 1.0mL min-1, detection wavelength of 254nm, and column temperature of 25 deg.C.
In one embodiment, the method for detecting a non-steroidal anti-inflammatory drug in a water sample comprises the following steps:
taking 5ml of water sample containing NSAIDs, and adjusting the pH value of the water sample to 5-10;
adding 5-30 mg of solid phase extraction material, carrying out vortex dispersion for 3-20 min, and carrying out magnetic separation to obtain a solid phase extraction product;
adding 100-800 mul of 2-6 mol/L acid solution, and dissolving the solid phase extraction product to obtain solution A;
adding 100-800 microliter SHS solution into the solution A, and performing homogeneous extraction to obtain extract B;
adding 100-400 mu L of alkaline solution with the concentration of 2-6 mol/L into the extract B, and inducing layering to obtain supernatant C;
and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
Firstly, enriching the non-steroidal anti-inflammatory drugs in a water sample by dispersive micro-solid phase extraction, then further enriching the non-steroidal anti-inflammatory drugs by adopting a homogeneous liquid-liquid micro-extraction method, and finally determining the content of the non-steroidal anti-inflammatory drugs by utilizing high performance liquid chromatography. Through the combination of dispersive micro-solid phase extraction, homogeneous phase liquid-liquid micro-extraction and high performance liquid chromatography, the sensitivity and selectivity of the detection of the non-steroidal anti-inflammatory drugs are improved, the analysis and detection time is greatly shortened to about 5min, the analysis and detection efficiency of the non-steroidal anti-inflammatory drugs in a water sample is improved, and in the analysis and detection process, only a certain amount of SHS solution is used to replace the traditional organic solvent, so that the method is green and environment-friendly.
It is worth mentioning that the nsaid includes one or more of Ketoprofen (KEP), Naproxen (NAP), and Tolmetin (TLM).
The technical scheme and technical effects of the invention are further explained by the specific examples below.
Example 1:
taking 10mg of Fe3O4The method comprises the following steps of adding @ ZnAl-LDH into 5mL of 5ng/mL simulated water sample containing NSAIDs, carrying out magnetic separation on the material after vortex for 5min, adding 200 mu L of HCl (4mol/L) solution to dissolve the magnetic material, then adding 100 mu L of triethylamine to be used as an SHS solution to carry out homogeneous extraction, finally adding 200 mu L of NaOH (2mol/L) solution to induce solution layering, taking 20 mu L of supernatant solution, and carrying out sample injection analysis by adopting high performance liquid chromatography.
The chromatographic conditions are as follows: the chromatographic column is an Agilent ZORBAX-C18 column (250mm × 4.6mm I.D.,5 μm); protection of the column: easy guard C18 guard column (8mm x 4mm i.d.,5 μm); the mobile phase is BNitrile-0.1% by mass hexanoic acid in water (68:32, v/v) was eluted with a gradient of 1.0mL min-1The detection wavelength is 254nm, and the column temperature is 25 ℃.
Referring to fig. 6, the total time of the above processes is 30min, wherein the time of the pretreatment process is only 10min, which greatly improves the extraction efficiency. The method has better detection rate and precision for the simulated water sample containing the NSAIDs with the concentration of 5 ng/mL.
Example 2:
taking 30mg of Fe3O4The method comprises the following steps of adding @ ZnAl-LDH into 5mL of 5ng/mL simulated water sample containing NSAIDs, performing magnetic separation on the material after swirling for 20min, adding 800 mu L of trifluoroacetic acid (2mol/L) solution to dissolve the magnetic material, adding 800 mu L of triethylamine as an SHS solution to perform homogeneous extraction, adding 400 mu L of NaOH (6mol/L) solution to induce solution layering, taking 20 mu L of supernatant solution, and performing sample injection analysis by adopting high performance liquid chromatography. The chromatographic conditions were the same as in example 1.
The total time of the processes is 40min, wherein the time of the pretreatment process is only 25min, and the extraction efficiency is greatly improved. The method has better detection rate and precision for the simulated water sample containing the NSAIDs with the concentration of 5 ng/mL.
Example 3:
taking 5mg of Fe3O4The method comprises the following steps of adding @ ZnAl-LDH into 5mL of 5ng/mL simulation water sample containing NSAIDs, carrying out magnetic separation on the material after swirling for 3min, adding 100 mu L of sulfuric acid (6mol/L) solution to dissolve the magnetic material, then adding 100 mu L of triethylamine to be used as an SHS solution to carry out homogeneous extraction, finally adding 100 mu L of NaOH (4mol/L) solution to induce solution layering, taking 20 mu L of supernatant solution, and carrying out sample injection analysis by adopting high performance liquid chromatography. The chromatographic conditions were the same as in example 1.
The total time of the processes is 20min, wherein the time of the pretreatment process is only 5min, and the extraction efficiency is greatly improved. The method has better detection rate and precision for the simulated water sample containing the NSAIDs with the concentration of 5 ng/mL.
Please refer to table 2, which compares the advantages and disadvantages of the disclosed method and the method provided by the present invention.
Table 2 comparison of other analytical methods reported in the open literature
In the table, D- μ -SPE: Dispersive micro-solid phase extraction (Dispersive micro-solid phase extraction)
SRSE, Stir rod adsorptive extraction
SPE Solid phase extraction
MSPE Magnetic solid phase extraction
ACN Acetonitrile (Acetonitrile); MeOH Methanol
As can be seen from the above table, compared with the technical solutions disclosed in the documents, the technical solution of the present invention significantly shortens the pre-treatment time, can quickly complete the extraction of the NSAIDs components of the simulated water sample containing NSAIDs within 5min, and improves the detection efficiency. Meanwhile, the lower detection limits of the non-steroidal anti-inflammatory drugs including Ketoprofen (KEP), Naproxen (NAP) and Tolmetin (TLM) are respectively 0.02ng/mL, 0.05ng/mL and 0.05ng/mL, which are improved compared with the published documents. Meanwhile, in the technical scheme provided by the invention, only the low-dose SHS solution is used in the detection process of the non-steroidal anti-inflammatory drug, so that the method is green and environment-friendly.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. A method for detecting non-steroidal anti-inflammatory drugs in a water sample is characterized by comprising the following steps:
dispersed micro solid phase extraction: adding the solid-phase extraction material into a water sample containing NSAIDs, and performing magnetic separation after full dispersion to obtain an extraction product;
acid hydrolysis: adding an acidic solution into the extraction product to dissolve the solid-phase extraction product to obtain a solution A;
homogeneous liquid-liquid microextraction: adding an SHS solution into the solution A to perform homogeneous liquid-liquid microextraction to obtain an extract B;
layering: adding an alkaline solution into the extract B, and inducing layering to obtain a supernatant C;
high performance liquid chromatography determination: and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
2. A method of detecting a non-steroidal anti-inflammatory drug in a water sample according to claim 1, comprising the steps of:
taking 5ml of water sample containing NSAIDs, and adjusting the pH value of the water sample to 5-10;
adding 5-30 mg of solid phase extraction material, carrying out vortex dispersion for 3-20 min, and carrying out magnetic separation to obtain a solid phase extraction product;
adding 100-800 mul of 2-6 mol/L acid solution, and dissolving the solid phase extraction product to obtain solution A;
adding 100-800 microliter SHS solution into the solution A, and performing homogeneous extraction to obtain extract B;
adding 100-400 mu L of alkaline solution with the concentration of 2-6 mol/L into the extract B, and inducing layering to obtain supernatant C;
and (4) determining the content of the NSAIDs in the supernatant C by adopting high performance liquid chromatography.
3. The method according to claim 1 or 2, wherein the solid phase extraction material is magnetic layered double hydroxide Fe3O4@ZnAl-LDH。
4. The method of claim 1 or 2, wherein the acidic solution is one of sulfuric acid, hydrochloric acid, nitric acid and trifluoroacetic acid.
5. The method according to claim 1 or 2, wherein the SHS solution is one of dipropylamine, triethylamine and N, N-dimethylcyclohexylamine.
6. A method as claimed in claim 1 or claim 2 wherein said alkaline solution is sodium hydroxide or potassium hydroxide.
7. The method for detecting NSAIDs in a water sample according to claim 1 or 2, wherein the "determination of NSAIDs content in supernatant C by HPLC" comprises the following chromatographic conditions:
the chromatographic column is an Agilent ZORBAX-C18 column (250mm × 4.6mm I.D.,5 μm); protection of the column: EasyGuard C18 guard column (8mm × 4mm I.D.,5 μm), acetonitrile-0.1% hexanoic acid aqueous solution (68:32, v/v) as mobile phase, and flow rate of 1.0 mL/min-1The detection wavelength is 254nm, and the column temperature is 25 ℃.
8. A method as claimed in claim 1 or claim 2 wherein the nsaid comprises one or more of ketoprofen, naproxen and tolmetin.
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| CN114487202A (en) * | 2022-02-14 | 2022-05-13 | 宁夏医科大学 | Detection method of SUHs in traditional Chinese medicinal materials |
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| CN1486690A (en) * | 2002-10-02 | 2004-04-07 | ����ҩƷ��ҵ�ɷ�����˾ | Medicinal salt with local narcosis and antiphlogosis activity and its prepn process |
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| CN1486690A (en) * | 2002-10-02 | 2004-04-07 | ����ҩƷ��ҵ�ɷ�����˾ | Medicinal salt with local narcosis and antiphlogosis activity and its prepn process |
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| MALEK HASSAN 等: "Switchable-hydrophilicity solvent liquid–liquid microextraction of non-steroidal anti-inflammatory drugs from biological fluids prior to toHPLC-DAD determination", 《JOURNAL OF PHARMACEUTICAL AND BIOMEDICAL ANALYSIS》 * |
| SHENG TANG 等: "Automated Dispersive Solid-Phase Extraction Using Dissolvable Fe3O4‑Layered Double Hydroxide Core−Shell Microspheres as Sorbent", 《ANAL. CHEM》 * |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114487202A (en) * | 2022-02-14 | 2022-05-13 | 宁夏医科大学 | Detection method of SUHs in traditional Chinese medicinal materials |
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