CN110231423A - The method of pyrethroid pesticide in dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain - Google Patents
The method of pyrethroid pesticide in dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain Download PDFInfo
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Abstract
The invention belongs to Food Chemistry technical fields, provide a kind of method that dispersive liquid-liquid microextraction-high performance liquid chromatography measures pyrethroid pesticide in grain.Using thymol or choline chloride as hydrogen bond receptor, as hydrogen bond donor, hydrogen bond receptor and hydrogen bond donor molar ratio are any one in 1/5,1/4,1/3,1/2,1/1,2/1,3/1 or 4/1 for valeric acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid or capric acid；The hydrophobicity eutectic solvent that hydrogen bond receptor mixes synthesis with donor makees extractant, carries out dispersive liquid-liquid microextraction, and high performance liquid chromatography measures pyrethroid pesticide in grain.Operation of the present invention is simple, rapid sensitive, extractant usage amount is few, is easy to the advantages that collecting, is environmentally protective, can be used for the detection of pyrethrin pesticide in plurality of cereals sample.Can be avoided using harmful organic solvent, and extractant usage amount is few, have it is easy to operate quickly, be easy to the significant advantages such as collection, environmentally protective, favorable reproducibility.
Description
Technical field
The invention belongs to Food Chemistry technical fields, and in particular to a kind of dispersive liquid-liquid microextraction-high performance liquid chromatography survey
Determine the method for pyrethroid pesticide in grain.
Background technique
Pyrethroid pesticide is simulation natural pyrethrum by an artificial synthesized insecticides, is mainly used for preventing and treating
Agricultural pests, but since it has a wide range of application, quantity is big, exposed population group is more, so poisoning case occurs repeatedly.Less serious case's headache,
There is muscle fibre trembling in nausea, serious person, or even with stupor and kidney function damage.And grain not only can satisfy our human bodies
Primary demand, can also prevent and assist in the treatment of many diseases, therefore the quality control of grain is extremely important.
Dispersive liquid-liquid microextraction is equivalent to the liquid-liquid extraction of micromation, and principle is extractant shape under the action of dispersing agent
It is a kind of simple and quick, at low cost to form water, dispersing agent, extractant emulsion system at tiny organic drop of dispersion
Sample-pretreating method honest and clean, enrichment times are high, the always deep concern by researchers.However, the common extractant of this method
It is unfavorable to operator and environment for organic solvent.Therefore select a kind of green extractant particularly important.
General technology based on the cured dispersive liquid-liquid microextraction that suspends is similar to traditional liquid-liquid dispersions micro-extraction, passes through
Dispersive liquid-liquid microextraction is carried out close to the extractant that room temperature, density are less than water using fusing point, by extraction container after being only centrifuged
It is put into ice bath and solidifies organic phase, to be conducive to the collection of extract, can easily collect separation without special device.The method
Have many advantages, such as that fast speed, favorable reproducibility, high-efficient, at low cost, extraction equipment is simple, low-toxic organic solvent dosage is few.
Summary of the invention
The object of the present invention is to provide pyrethroids in a kind of dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain
The method of class pesticide.This method has that easy to operate, rapid sensitive, extractant usage amount is few, is easy to collect, is environmentally protective etc. excellent
Point can be used for the detection of pyrethrin pesticide in plurality of cereals sample.
The present invention designs for the first time uses a kind of novel hydrophobicity eutectic solvent, the extraction as dispersive liquid-liquid microextraction
Agent is taken, is aided with suspension solidification and is collected, pyrethroid pesticide in grain is measured point in conjunction with high performance liquid chromatography
Analysis.
The present invention is realized by following technical solution: in a kind of dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain
The method of pyrethroid pesticide, using thymol or choline chloride as hydrogen bond receptor, valeric acid, caproic acid, enanthic acid, octanoic acid,
As hydrogen bond donor, the molar ratio of hydrogen bond receptor and hydrogen bond donor is 1/5,1/4,1/3,1/2,1/1,2/1,3/ for n-nonanoic acid or capric acid
Any one in 1 or 4/1；The hydrophobicity eutectic solvent of synthesis is mixed using hydrogen bond receptor with hydrogen bond donor as extractant,
Dispersive liquid-liquid microextraction is carried out, pyrethroid pesticide in high performance liquid chromatography measurement grain is then carried out.
Specific measuring method are as follows:
(1) it prepares sample solution: accurately weighing 1~5 g of grain samples to be measured after crushing homogeneous, be accurate to 0.0001 g, add
Enter the dispersing agent of the mL of 0.2 mL~1.2, and with 1000~3500 r/min vortex mixed, 3~10 min, takes out supernatant, to
With；
(2) it collects extract liquor: the hydrophobicity eutectic solvent of 40 mL of μ L~1 being added in supernatant obtained by step (1), after extraction
5~15 min are centrifuged with 2500~5000 r/min, are subsequently placed in the ice bath for carrying out 10~150 min in refrigerator, phase to be extracted
After being converted into solid phase, melting at room temperature is liquid, is collected with glass syringe absorption；
(3) high effective liquid chromatography for measuring is analyzed: by standard solution obtained and testing sample solution setting liquid chromatogram
Under the conditions of sample introduction measure, according to the chromatogram peak area of sample to be tested and combine pyrethrin pesticide concentration correspond to chromatogram peak out face
Long-pending standard curve realizes the quantitative detection of pyrethrin pesticide in sample to be tested.
The grain samples to be measured are at least one of corn, wheat, barley, sorghum, rice, oat, rye；It is described
Pyrethrin pesticide is Biphenthrin, effective cypermethrin, any one in decis.
The dispersing agent is methanol, acetonitrile, any one in acetone；The volume of the dispersing agent is 0.4 mL~1.1
mL；The extractant is made by thymol is mixed with octanoic acid, n-nonanoic acid or capric acid；The volume of the extractant be 40 μ L~
100 μL。
Thymol-the octanoic acid is 1/4 mixing as extractant using molar ratio, and extractant volume is 60 μ L.Described point
Powder is acetonitrile, and volume is 0.8 mL.
The vortex time is 3~8 min；Revolving speed is 1500~3000 r/min.
7~13 min are centrifuged after extracting in step (2) with 3500~4500 r/min.The ice bath time in the refrigerator is
10~40 min.
The actual conditions of high effective liquid chromatography for measuring are as follows in step (3): mobile phase A: the acetonitrile that B is 95%: 5%
Water, flow velocity are 0.5 mL/min, and sample volume is 20 μ L, and Detection wavelength is 220 nm；Every time before use, with mobile phase acetonitrile/water
Rinse pillar at least 30 min.
It is used for the first time in the present invention using thymol-octanoic acid synthesis hydrophobicity eutectic solvent as extractant, tool
Have it is at low cost, easy to operate quickly, be easy to the significant advantages such as collection, environmentally protective, favorable reproducibility.Because prepared by eutectic solvent
Selected materials are mostly the already existing substance of nature, so most eutectic solvent can biodegrade.Therefore, it adopts
With eutectic solvent, the use of harmful organic solvent is avoided, reduces adverse effect and damage to ecological environment, it is greener
Colour circle is protected.The eutectic solvent studied at present be mostly it is hydrophilic, due to hydrogen bond action, be subject to destroy in water.It opens
Hair hydrophobicity eutectic solvent will greatly widen the application range of eutectic solvent.
Hydrophobicity eutectic solvent has the characteristics that low-freezing, since its freezing point is close to room temperature (10-30 DEG C),
It can be solidified.Eutectic solvent is subjected to ice bath at a certain temperature, make it with solid suspension in test tube upper end and is incited somebody to action
It is collected.This greatly reduces the collection difficulty of extract, reduce loss, keep experimental implementation also easier.In addition, this
The usage amount pettiness of extractant in invention, it is only necessary to which 60 μ L have greatly saved extraction agent dose.
Whole experiment process is easy to operate, rapid sensitive, has and avoids using organic solvent, saves extractant dosage, easily
In the advantages such as collection, environmentally protective.The present invention illustrates the method for the present invention suitable for grain by the rate of recovery and Precision Experiment
The quality of pyrethroid pesticide content controls.
Detailed description of the invention
Fig. 1 is influence of the extractant type to extraction efficiency in the present invention.
Fig. 2 is influence of the extractant component ratio to extraction efficiency in the present invention.
Fig. 3 is influence of the extractant volume to extraction efficiency in the present invention.
Fig. 4 is influence of the dispersing agent volume to extraction efficiency in the present invention.
Fig. 5 is influence of the additive amount of salt in the present invention to extraction efficiency.
Specific embodiment
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
In following embodiments, Biphenthrin, effective cypermethrin, the standard items of decis, sodium chloride, acetonitrile, methanol,
Thymol, octanoic acid, n-nonanoic acid, capric acid are bought in Shanghai Aladdin biochemical technology limited liability company.Corn, wheat, barley,
Sorghum, rice, oat, rye are all from Agricultural University Of Shanxi.It is mixed using the standard inventory that standard items prepare 3 kinds of objects
Liquid, and saved.
1260 high performance liquid chromatograph of Agilent (agilent company)；Eclipse Plus C18 chromatographic column (250
× 4.6mm, 5 μm)；SC-3610 low speed centrifuge (Anhui Zhong Kezhongjia Instrument Ltd.)；Electronic balance (Ao Haosi instrument
(Changzhou) Co., Ltd)；Refrigerator；Vortex instrument.
The method of pyrethroid pesticide, specific implementation in dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain
Steps are as follows:
(1) preparation of sample solution: 1 g of grain samples to be measured after crushing homogeneous is accurately weighed in 10 mL centrifuge tubes, is added
2 mL acetonitriles promote to extract, it is molten as sample to take out supernatant using the vortex auxiliary that the revolving speed of 2500 r/min carries out 5 min
Liquid-liquid micro-extraction process after liquid progress；
(2) it extracts collection process: the aqueous solution of 5 mL being taken to be placed in the centrifuge tube of 10 mL, the above-mentioned acetonitrile solution of 0.8 mL is added,
Eutectic solvent made of thymol-octanoic acid that 60 μ L molar ratios are 1/4 is mixed with, mixes well.Then with 4000
R/min is centrifuged 10 min, and the fine drop for dispersing extraction phase swims in tube top.Centrifuge tube is subjected to ice bath about 10-20 later
Min, inversion of phases to be extracted are liquid to melt after solid phase at room temperature, are drawn with the glass syringe of 50 μ L, dilute with methanol
Release sample introduction；
(3) high effective liquid chromatography for measuring is analyzed: by standard solution obtained and testing sample solution setting liquid chromatogram
Under the conditions of sample introduction measure, according to the chromatogram peak area of sample to be tested and combine pyrethrin pesticide concentration correspond to chromatogram peak out face
Long-pending standard curve realizes the quantitative detection of pyrethrin pesticide in sample to be tested.
The actual conditions of high effective liquid chromatography for measuring are as follows: mobile phase is 95% acetonitrile (A) and 5% water (B), flow velocity
For 0.5 mL/min, sample volume is 20 μ L, and Detection wavelength is 220 nm.Every time before use, rinsing pillar at least with acetonitrile/water
30 min。
Experimental result is as follows:
Linear and detection limit: linearity curve is to be mapped with corresponding various material concentrations by peak area and obtained.The method is intended removing to 3 kinds
The linearity of worm pyrethroids is all fine, is all larger than 0.9997, detection is limited to 2.95-4.00 μ g/kg.
Extraction process optimization: it is tested according to above-mentioned experimental procedure using different extractants, extractant is specific as follows:
Thymol-octanoic acid, thymol-n-nonanoic acid, thymol-capric acid (three 1/4 prepares in molar ratio).Experimental result is as schemed
Shown in 1, three's rate of recovery is higher, does not have significant difference to the extraction efficiency of all analytes.But due to thymol-
N-nonanoic acid curing time needs 2.5 h or so, greatly extends experimental period, is not suitable for practical operation.We are at other two kinds
It is middle to select thymol-octanoic acid as extractant.
The extractant of different mol ratio example (1/5,1/4,1/3,1/2,1/1,2/1,3/1) is used according to above-mentioned experimental procedure
It is tested.As a result as shown in Fig. 2, the eutectic solvent of different mol ratio has active influence to the extraction of analyte.Mole
The eutectic solvent obtained when than being 1/4 has higher extraction efficiency than other molar ratios.Therefore, thymol and octanoic acid
Optimum proportioning is 1/4.
It is tested according to above-mentioned experimental procedure using the extractant of different volumes (40 μ of μ L~100 L).As a result such as Fig. 3
Shown, as the volume of eutectic solvent increases to 60 μ L from 40 μ L, the enrichment times of pyrethrin pesticide increase, extraction efficiency
It is gradually increased, when eutectic solvent volume increases to 100 μ L from 60 μ L, extraction efficiency is in basicly stable trend.It should infuse
Meaning, when volume is less than 40 μ L, volume is too small, it is extremely difficult to collect and handle.Accordingly, it is considered to fact of case and experimental result, choosing
Select volume of the 60 μ L as extractant.
It is tested according to above-mentioned experimental procedure using the dispersing agent acetonitrile of different volumes (mL of 0.4 mL~1.1).As a result
As shown in figure 4, the volume when acetonitrile increases to 0.8 mL from 0.4 mL, extraction efficiency is in rising trend.This is because dispersing agent
The increase of volume makes dispersion effect improve, and the extraction efficiency of extract increases with it.But when the volume of acetonitrile increases from 0.8 mL
To 1.1 mL, since dispersing agent is using excessively, the solubility increase of analyte in water is not easy to be extracted, therefore extraction efficiency subtracts
It is small.So selecting 0.8 mL as optimal dispersing agent volume.
It is tested according to above-mentioned experimental procedure using the salt of Different adding amount (g of 0 g~1.5).As shown in figure 5,0
The increase of salt additive amount gradually decreases extraction efficiency in the range of g-1.5 g, and when 0 g salt, extraction efficiency reaches highest.This
As a result it can be construed to, due to the chloride ion and hydrogen bond donor formation hydrogen bond in solution, thymol-octanoic acid may be destroyed
Extractant causes recovery of extraction to reduce.Therefore, next experiment is carried out in the case where not adding salt.
Actual sample detection: it is removed according to above-mentioned experimental procedure to quasi- in 4 kinds of grain samples (corn, wheat, barley, oat)
Worm pyrethrin pesticide is analyzed.Extraction concentration is 0.25 mg kg at optimum conditions-1、 2.5 mg kg -1With 25 mg
kg-1Three kinds of grain samples solution.All samples are triplicate, carry out the calculating rate of recovery using external standard method, as a result such as 1 institute of table
Show.
The rate of recovery of 1 four kinds of samples of table
Claims (10)
1. the method for pyrethroid pesticide, feature in a kind of dispersive liquid-liquid microextraction-high performance liquid chromatography measurement grain
Be: using thymol or choline chloride as hydrogen bond receptor, valeric acid, caproic acid, enanthic acid, octanoic acid, n-nonanoic acid or capric acid are as hydrogen bond
The molar ratio of donor, hydrogen bond receptor and hydrogen bond donor is any one in 1/5,1/4,1/3,1/2,1/1,2/1,3/1 or 4/1
Kind；The hydrophobicity eutectic solvent of synthesis is mixed using hydrogen bond receptor with hydrogen bond donor as extractant, carries out the micro- extraction of dispersion liquid
It takes, then carries out pyrethroid pesticide in high performance liquid chromatography measurement grain.
2. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 1-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: specific measuring method are as follows:
(1) it prepares sample solution: accurately weighing 1~5 g of grain samples to be measured after crushing homogeneous, be accurate to 0.0001 g, add
Enter the dispersing agent of the mL of 0.2 mL~1.2, and with 1000~3500 r/min vortex mixed, 3~10 min, takes out supernatant, to
With；
(2) it collects extract liquor: the hydrophobicity eutectic solvent of 40 mL of μ L~1 being added in supernatant obtained by step (1), after extraction
5~15 min are centrifuged with 2500~5000 r/min, are subsequently placed in the ice bath for carrying out 10~150 min in refrigerator, phase to be extracted
After being converted into solid phase, melting at room temperature is liquid, is collected with glass syringe absorption；
(3) high effective liquid chromatography for measuring is analyzed: by standard solution obtained and testing sample solution setting liquid chromatogram
Under the conditions of sample introduction measure, according to the chromatogram peak area of sample to be tested and combine pyrethrin pesticide concentration correspond to chromatogram peak out face
Long-pending standard curve realizes the quantitative detection of pyrethrin pesticide in sample to be tested.
3. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the grain samples to be measured are corn, wheat, barley, sorghum, rice, oat, rye
At least one of；The pyrethrin pesticide is Biphenthrin, effective cypermethrin, any one in decis.
4. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the dispersing agent is methanol, acetonitrile, any one in acetone；The body of the dispersing agent
Product is the mL of 0.4 mL~1.1；The extractant is made by thymol is mixed with octanoic acid, n-nonanoic acid or capric acid；The extractant
Volume be 40 μ of μ L~100 L.
5. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 4-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the thymol-octanoic acid is mixed for 1/4 as extractant, extractant body using molar ratio
Product is 60 μ L.
6. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 4-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the dispersing agent is acetonitrile, and volume is 0.8 mL.
7. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the vortex time is 3~8 min；Revolving speed is 1500~3000 r/min.
8. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: be centrifuged 7~13 min after extracting in step (2) with 3500~4500 r/min.
9. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the ice bath time in the refrigerator is 10~40 min.
10. pyrethroid in a kind of dispersive liquid-liquid microextraction according to claim 2-high performance liquid chromatography measurement grain
The method of class pesticide, it is characterised in that: the actual conditions of high effective liquid chromatography for measuring are as follows in step (3): mobile phase A: B is
95% acetonitrile: 5% water, flow velocity are 0.5 mL/min, and sample volume is 20 μ L, and Detection wavelength is 220 nm；Every time before use,
Pillar at least 30 min are rinsed with mobile phase acetonitrile/water.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111034718A (en) * | 2019-12-20 | 2020-04-21 | 中国农业大学 | Liquid pesticide preparation and preparation method thereof |
| CN111679024A (en) * | 2020-07-21 | 2020-09-18 | 甘肃省食品检验研究院 | Preparation of hydrophobic low-temperature eutectic and method for extracting Congo red, acid golden yellow and red 2G in meat products and aquatic products |
| CN111735883A (en) * | 2020-07-03 | 2020-10-02 | 呼和浩特海关技术中心 | Method for detecting phenylbutazone in horse meat based on eutectic solvent |
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| CN114354323A (en) * | 2022-01-17 | 2022-04-15 | 山西农业大学 | Method for determining parathion in grain by combining dispersion liquid-liquid microextraction with digital image colorimetry based on hydrophilic and hydrophobic eutectic solvents |
| CN114577952A (en) * | 2022-04-13 | 2022-06-03 | 河南师范大学 | Method for enriching and determining antiviral drug famciclovir residue in environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
| CN103926362A (en) * | 2014-04-24 | 2014-07-16 | 江苏太湖地区农业科学研究所 | Quantitative detection method for pyrethriods pesticide in soil |
| CN106290673A (en) * | 2016-09-27 | 2017-01-04 | 深圳市计量质量检测研究院 | A kind of method that eutectic solvent extract phase chromatography quickly measures rhodamine B |
| CN108572231A (en) * | 2018-06-26 | 2018-09-25 | 河南师范大学 | The method of hydrophobicity eutectic solvent vortex aid dispersion liquid-liquid micro-extraction-high performance liquid chromatography detection Sudan red 1 |
| CN109115898A (en) * | 2018-06-14 | 2019-01-01 | 浙江工业大学 | Based on the remaining method of pesticide in eutectic solvent-inorganic salts double-aqueous phase system analysis water-like |
-
2019
- 2019-07-05 CN CN201910602136.2A patent/CN110231423B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101915809A (en) * | 2010-07-01 | 2010-12-15 | 王冬群 | Detection method of pyrethroid pesticide remained in rice |
| CN103926362A (en) * | 2014-04-24 | 2014-07-16 | 江苏太湖地区农业科学研究所 | Quantitative detection method for pyrethriods pesticide in soil |
| CN106290673A (en) * | 2016-09-27 | 2017-01-04 | 深圳市计量质量检测研究院 | A kind of method that eutectic solvent extract phase chromatography quickly measures rhodamine B |
| CN109115898A (en) * | 2018-06-14 | 2019-01-01 | 浙江工业大学 | Based on the remaining method of pesticide in eutectic solvent-inorganic salts double-aqueous phase system analysis water-like |
| CN108572231A (en) * | 2018-06-26 | 2018-09-25 | 河南师范大学 | The method of hydrophobicity eutectic solvent vortex aid dispersion liquid-liquid micro-extraction-high performance liquid chromatography detection Sudan red 1 |
Non-Patent Citations (3)
| Title |
|---|
| HUAZI WANG等: "Deep eutectic solvent-based ultrasound-assisted dispersive liquid-liquid microextraction coupled with HPLC for the determination of ultraciolet filters in water samples", 《JOURNAL OF CHROMATOGRAPHY A》 * |
| XINYA LIU等: "Ulteasound-assisted dispersive liquid-liquid microextraction based on a hydrophobic deep eutectic solvent for the preconcentration of pyrethroid insecticides prior to determination by HPLC", 《MICROCHEMICAL JOURNAL》 * |
| 张盈盈等: "胆碱类低共熔溶剂的物性及应用", 《化学进展》 * |
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| CN113203720A (en) * | 2021-06-15 | 2021-08-03 | 山西农业大学 | Method for detecting residual amount of dichlorvos in aquatic product by fluorescence analysis method and detection kit |
| CN113866115A (en) * | 2021-10-25 | 2021-12-31 | 重庆食品工业研究所有限公司 | Method for detecting cadmium in food |
| CN114354805A (en) * | 2021-12-31 | 2022-04-15 | 山西大学 | MOF-based SPME-DLLME-HPLC-MS method for detecting pesticide in food and application |
| CN114354805B (en) * | 2021-12-31 | 2023-11-14 | 山西大学 | MOF-based SPME-DLLME-HPLC-MS method for detecting insecticide in food and application |
| CN114354323A (en) * | 2022-01-17 | 2022-04-15 | 山西农业大学 | Method for determining parathion in grain by combining dispersion liquid-liquid microextraction with digital image colorimetry based on hydrophilic and hydrophobic eutectic solvents |
| CN114577952A (en) * | 2022-04-13 | 2022-06-03 | 河南师范大学 | Method for enriching and determining antiviral drug famciclovir residue in environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction |
| CN114577952B (en) * | 2022-04-13 | 2023-08-04 | 河南师范大学 | Method for determining antiviral drug famciclovir residue in environmental water sample based on hydrophobic eutectic solvent liquid-liquid microextraction enrichment |
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