CN109856284A - Imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma - Google Patents
Imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma Download PDFInfo
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Abstract
The present invention relates to imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma, include the following steps: dog or cat plasma sample pre-treatment: acetonitrile is added to dog, cat plasma sample, is centrifuged after mixing；It takes supernatant to be dried with nitrogen in 40 DEG C of sand-baths, obtains residue；Mobile phase solution is added in residue, redissolves, centrifugation, takes supernatant, filtrate is obtained by filtration；High performance liquid chromatography detection: Detection wavelength: 270 nm；Mobile phase: acetonitrile: ultrapure water；In mobile phase, acetonitrile, ultrapure water volume ratio are 26:74.The present invention only passes through acetonitrile extraction and cleaning, and nitrogen blows the imidacloprid in concentration plasma sample, is a kind of pre-treating method effectively, economic and easy.The peak shape at imidacloprid medicine peak is effectively improved, medicine peak retention time is stabilized, improves the drug rate of recovery.High-efficiency liquid chromatography method for detecting linear relationship in the present invention is good, and stability is high, favorable reproducibility, and sensitive efficient, the rate of recovery is high.
Description
Technical field
The present invention relates to field of veterinary drug residue detection, and in particular to imidacloprid high performance liquid chromatography inspection in a kind of dog cat blood plasma
Survey method.
Background technique
The structure of imidacloprid is the combination of nicotine and Nitromethylene heterocycle structure, belongs to chlorination nicotinic insecticide.This is killed
Worm agent be improve using natural nicotine as model through structure made of, there is the mechanism of action identical with natural nicotine.It is characterized in that
With low dosage, efficiently and environmental safety, while the drug alternative is in conjunction with the acetylcholinergic receptor of insect, without with
The acetylcholinergic receptor of mammal combines, and has good selectivity and application prospect.In China imidacloprid be usually used in cotton,
Primary pest on rice, wheat, vegetables and each planting fruit-trees.Therefore in China, high performance liquid chromatography is used to crops, soil at present
Imidacloprid detection in earth, vegetables and fruit, and when measuring imidacloprid content, sample pre-treatments are complicated, and repeatedly extraction is needed to turn
It moves, is purified through gel permeation chromatography, analysis cost is high, and step is more and be easy to cause loss, and the rate of recovery is low, but has no in dog cat blood
Imidacloprid high-efficiency liquid chromatography method for detecting in slurry.
With the rapid development of Chinese pet quantity, the infection of pet pulicosis increases rapidly.External application anthelmintic has become treatment
The prefered method of pet pulicosis.Imidacloprid has a good killing effect for the insect of the tool sucking mouth parts such as flea class, but in view of
When imidacloprid is as dog cat external application anthelmintic, the current country there is no pertinent literature to report.
Summary of the invention
For the technological gap for the imidacloprid high-efficiency liquid chromatography method for detecting filled up in dog cat blood plasma, the present invention provides one
Imidacloprid high-efficiency liquid chromatography method for detecting in kind dog cat blood plasma, this method effectively improve the peak shape at imidacloprid medicine peak, stablize
Medicine peak retention time, improves the drug rate of recovery.High-efficiency liquid chromatography method for detecting by methodological study, in the present invention
Linear relationship is good, and stability is high, favorable reproducibility, and sensitive efficient, the rate of recovery is high.
In order to achieve the above-mentioned object of the invention, the technical solution adopted by the present invention are as follows: imidacloprid is efficient in a kind of dog cat blood plasma
Liquid chromatography detecting method includes the following steps:
1) dog or cat plasma sample pre-treatment:
Acetonitrile is added to dog, cat plasma sample, is centrifuged after mixing；It takes supernatant to be dried with nitrogen in 40 DEG C of sand-baths, obtains residual
Slag；Mobile phase solution is added in residue, redissolves, centrifugation, takes supernatant, filtrate is obtained by filtration；
2) high performance liquid chromatography detection:
Chromatographic column:C18；Detector: UV detector；Column temperature: 35 DEG C；Detection wavelength: 270nm；Sample flow
Speed: 1mL/min；Mobile phase: acetonitrile: ultrapure water；In mobile phase, acetonitrile, ultrapure water volume ratio are 26:74.
Imidacloprid high-efficiency liquid chromatography method for detecting (dog, cat method are consistent) in a kind of dog cat blood plasma, including apparatus selection,
Setting, plasma sample sample pretreatment and the upper machine testing of chromatographic condition.Liquid chromatograph used in the present invention are as follows: efficient liquid
The 2695 reciprocating pumps in series of constant current mode double plunger (Waters, USA) of chromatography Waters.
Chromatographic condition are as follows: chromatographic column:C18 (250mm × 4.6mm, 5 μm)；Detector: UV detector
2998 diode array detector of Waters, 3 work station of Empower (Waters, USA)；Column temperature: 35 DEG C；Detection wavelength:
270nm；Sample volume: 10 μ L；Flow velocity: 1mL/min；Mobile phase: acetonitrile: ultrapure water (V:V)=26:74.
Plasma sample pre-treating method: taking 200 μ L of plasma sample, be placed in 2mL EP pipe, and acetonitrile 1mL → vortex is added
3min, ultrasonic 3min, 4 DEG C of 12000r/min centrifugation 10min → supernatant is drawn in 10mL EP pipe with pipettor, in 40 DEG C
Be dried with nitrogen in sand-bath → 200 μ L of mobile phase solution is added in residue, vortex oscillation 3min → by the solution after redissolution moves to 1.5mL
In EP pipe, centrifugation 10min (4 DEG C, 12000r/min) → take supernatant through 0.22 μm of organic membrane filtration and → filtrate confession of bottling
HPLC analysis.
1. chromatographic condition optimizes
Spectral scan is carried out to imidacloprid standard solution in the range of 200~400nm wavelength, discovery imidacloprid is maximum
UV absorption wavelength is 270nm, therefore selects 270nm as Detection wavelength in HPLC analysis.The stream of imidacloprid HPLC detection method
Dynamic phase is generally made of organic phase (methanol) and water phase (ultrapure water).This experiment has been respectively compared methanol and acetonitrile as mobile phase
The response of drug when B can preferably separate drug as the result is shown, but when acetonitrile is as organic phase, target peak performance more preferably,
Therefore the mobile phase of this experiment, using acetonitrile as organic phase, ultrapure water is as water phase.The study find that in mobile phase acetonitrile with it is ultrapure
The volume ratio of water is affected to imidacloprid peak retention time.It is found through test of many times: when the volume ratio of acetonitrile and ultrapure water
When for 26:74, the chromatographic peak retention time of imidacloprid standard items is 7.9min, is 7.7min in plasma sample, and target peak with
Impurity peaks separation in plasma sample is preferable.
2. plasma sample pre-treatment optimizes
The pretreated key point of plasma sample is the removal of protein.Method includes: addition organic solvent, column such as first
Alcohol, second eyeball, tetrahydrofuran, acetone etc.；Neutral salt, such as phosphate, ammonium acetate etc. is added；Strong acid is added；Be added containing zinc salt with
And mantoquita；Enzymatic isolation method etc..And the common extractant of imidacloprid includes: acetonitrile, methylene chloride, methanol etc. in blood plasma.This experiment point
It does not compare and extracts pyrrole in blood plasma using 1mL acetonitrile, 1mL methylene chloride, 1mL methanol and 1mL acetonitrile and 1mL methanol double solvents
The effect of worm quinoline.As the result is shown: after methylene chloride extracts, the rate of recovery is lower；After methanol extracts, the rate of recovery is lower；Methanol acetonitrile
After mixing is extracted, impurity serious interference；After being extracted using pure acetonitrile, the rate of recovery is high and impurity does not cause to do to imidacloprid chromatographic peak
It disturbs.Therefore select extractant of the acetonitrile as imidacloprid in blood plasma.This experiment removes extracting solution using the method that nitrogen is blown, and reaches concentration
The effect of drug target.Through repetition test, the rate of recovery that imidacloprid in plasma sample can be improved is blown using nitrogen, can prevent chromatographic column
The case where pollution, blocking, occurs.
Compared with the existing technology, the invention has the benefit that
Only by acetonitrile extraction and cleaning in the present invention, nitrogen blows the imidacloprid in concentration plasma sample, is a kind of effective, economical
With easy pre-treating method.The peak shape at imidacloprid medicine peak is effectively improved, medicine peak retention time is stabilized, drug is improved and returns
Yield.By methodological study, the high-efficiency liquid chromatography method for detecting linear relationship in the present invention is good, and stability is high, reappears
Property it is good, it is sensitive efficiently, the rate of recovery is high.
High-efficiency liquid chromatography method for detecting in through the invention can carry out imidacloprid the intracorporal pharmacokinetics of dog cat,
The research such as Bioequivalence Test.For imidacloprid it is safer, effective for the pets clinic pulicosis such as dog cat treatment foundation is provided, it is right
China's pet diagnosis and treatment industry has important clinical significance and broad mass market prospect.
Detailed description of the invention
The chromatogram of Fig. 1 imidacloprid standard items；
The chromatogram of Fig. 2 dog blank plasma；
Fig. 3 dog blank plasma adds the chromatogram of imidacloprid (10 μ g/mL)；
The chromatogram of Fig. 4 cat blank plasma；
Fig. 5 cat blank plasma adds the chromatogram of imidacloprid (10 μ g/mL)；
Fig. 6 HPLC detects the standard curve of imidacloprid in cat blood plasma；
Fig. 7 HPLC detects the standard curve of imidacloprid in dog plasma.
Specific embodiment
Term as used in the present invention generally has those of ordinary skill in the art usual unless otherwise specified
The meaning of understanding.
Combined with specific embodiments below, and referring to data the present invention is described in further detail.These embodiments only be
It illustrates the present invention, rather than limits the scope of the invention in any way.
Below in an example, the various processes and method being not described in detail are conventional methods as known in the art.
The source of agents useful for same, trade name and it is necessary to list its constituent person, are indicated on the first occurrence, thereafter phase used
Unless otherwise specified with reagent, it is the same as indicated for the first time.
1. instrument of the present invention and consumptive material:
Waters series of high efficiency liquid chromatograph (the 2695 reciprocating pumps in series of constant current mode double plunger of Waters, Waters
2998 diode array detector, 3 work station of Empower)；
KQ-500E type ultrasonic cleaner: Kunshan Ultrasonic Instruments Co., Ltd.；
DHC-9140A type electric heating constant-temperature blowing drying box: the upper macro experimental facilities Co., Ltd of Nereid；
Eppendorf 5810R Centrifuge high speed freezing centrifuge: German Eppendorf company；
FA-2004 type electronic analytical balance: upper Nereid section balance；
KS-250D type ultrasonic cleaner: Ningbo Ke Sheng instrument plant.
Adjustable pipette: 20 μ L, 100 μ L, 200 μ L, 1000 μ L, 5000 μ L, German Eppendorf company；
SI adjustable speed eddy mixer VORTEX-GENIE2: Shanghai Si Baiming experimental instruments and equipment limited；
Nitrogen evaporator: Organomation company, the U.S.；
Organic phase pin type filter: 0.22 μm of aperture, the general experiment Science and Technology Co., Ltd. of Town in Shanghai.
0.45 μm of organic phase phase filter membrane, Shanghai peninsula Industrial Co., Ltd..
10mL dactylethrae, Yangtze glass for chemical equipment-building Instrument Ltd.；
1.5mL dactylethrae, Axygen company, the U.S..
2. test reagent used in the present invention:
Imidacloprid standard items are purchased from Dr.Ehrensterfer company, Germany；
Acetonitrile (chromatographically pure) is purchased from Sinopharm Chemical Reagent Co., Ltd..
3. main agents are prepared:
The preparation of imidacloprid titer:
Precision weighs imidacloprid reference substance about 5mg in 50mL volumetric flask, and with the dissolution of second eyeball and constant volume, that is, being made into concentration is
The quasi- stock solution of imidacloprid of 100 μ g/mL.
The preparation of standard working solution:
Appropriate imidacloprid standard reserving solution is accurately measured, with dilution in acetonitrile at series standard working solution.It is ready-to-use.
4. plasma sample pre-treating method:
Each 200 μ L of dog, cat plasma sample is taken, is placed in 2mL EP pipe, acetonitrile 1mL → vortex 3min, ultrasonic 3min is added,
4 DEG C of 12000r/min centrifugation 10min → supernatant is drawn in 10mL EP pipe with pipettor, are dried with nitrogen in 40 DEG C of sand-baths
200 μ L of mobile phase solution, vortex oscillation 3min → move to the solution after redissolution in 1.5mL EP pipe, centrifugation is added in → residue
10min (4 DEG C, 12000r/min) → take supernatant 0.22 μm of organic membrane filtration and bottled → and filtrate analyzes for HPLC.
5. chromatographic condition:
Detector: diode array detector；
Chromatographic column:C18 (250mm × 4.6mm, 5 μm)
Detector: UV detector
Column temperature: 35 DEG C
Detection wavelength: 270nm
Sample volume: 10 μ L
Flow velocity: 1mL/min
Mobile phase: acetonitrile: ultrapure water (V:V)=26:74
6. chromatographic behavior
The chromatogram of Fig. 1 imidacloprid standard items；
The chromatogram of Fig. 2 dog blank plasma；
Fig. 3 dog blank plasma adds the chromatogram of imidacloprid (10 μ g/mL)；
The chromatogram of Fig. 4 cat blank plasma；
Fig. 5 cat blank plasma adds the chromatogram of imidacloprid (10 μ g/mL).
7. linear relationship is investigated
Imidacloprid standard reserving solution is diluted to 100.0,20.0,10.0,5.0,1.0,0.5 with HPLC grades of acetonitrile solution
μ g/mL standard working solution draws each concentration standard working solution of 20 μ L in the EP pipe of 1.5mL respectively, and sequentially adds 180 μ L
Dog, cat blank plasma are diluted to the standard solution of 10.0,2.0,1.0,0.5,0.1,0.05 μ g/mL, use 4. blood later
After the processing of slurry samples pre-treating method, finally under 5. chromatographic conditions, sample introduction is distinguished by the sequence of concentration from low to high, is carried out
HPLC analysis.Quantified by external standard method, using concentration of standard solution as independent variable, using HPLC method measure the peak area of each concentration standard liquid as because
Variable is drawn peak area-concentration curve (such as Fig. 6 and Fig. 7), obtains equation of linear regression, cat: y=50068x+126.02 phase relation
Number R2=0.9999；Dog: y=50530x-762.88 coefficient R2=0.9999.It can be seen that linear relationship is good.8. inspection
Survey line and quantitative line measurement
By concentration be 0.8,0.5,0.4,0.3,0.1 μ g/mL imidacloprid standard working solution, 20 μ L, be separately added into 180 μ L dogs,
In cat blank plasma, so that imidacloprid content is 0.08,0.05,0.04,0.03,0.01 μ g/mL in dog, cat blank plasma.Into
Promoting circulation of blood slurry samples pre-treatment, supernatant carry out HPLC measurement.Baseline noise value is measured, is required, is won the confidence according to Ministry of Agriculture's test specification
Concentration when making an uproar than S/N >=3 is quantitative limit (LOQ)=0.05 μ g/ when being detection limit (LOD)=0.03 μ g/mL, S/N >=10
mL。
9. TIANZHU XINGNAO Capsul
Preparation concentration be 100.0,10.0,0.5 μ g/mL standard working solution, draw 20 μ L standard working solutions respectively, respectively plus
Enter into 180 μ L dogs and cat blank plasma, so that imidacloprid concentration is respectively 10.0,1.0,0.05 μ g/mL in dog, cat blood plasma.
After handling using 4. plasma sample pre-treating methods, supernatant is taken to carry out HPLC measurement, each concentration handles 5 in parallel respectively.
The standard curve for counting the peak area value of each concentration standard working solution measured, and it successively being substituted into the same day acquire survey it is dense
Degree.And calculate the rate of recovery (the results are shown in Table 1,2): imidacloprid blank plasma pitch-based sphere is in 0.05~10 μ g/mL, the rate of recovery
(cat) is between 89.75%~102.06%；The rate of recovery (dog) is between 85.85%~106.19%.
1 imidacloprid cat blank plasma of table adds sample recovery rate measurement result
2 imidacloprid dog blank plasma of table adds sample recovery rate measurement result
10. precision
The imidacloprid standard work for being 100.0,10.0,0.5 μ g/mL at concentration by imidacloprid standard reserving solution dilution in acetonitrile
Make each 20 μ L of liquid in the dog of 180 μ L, cat blank plasma, so that imidacloprid content is 10.0,1.0,0.05 μ in dog, cat blood plasma
g/mL.After handling using 4. plasma sample pre-treating methods, HPLC measurement is carried out.Each concentration samples are the same as in a few days replication 5
It is secondary, find out the in a few days coefficient of variation.In one week not on the same day to three concentration samples replication 3 times, find out the coefficient of variation in the daytime.
It the results are shown in Table 3,4.Imidacloprid blank plasma pitch-based sphere is in 0.05~10.0 μ g/mL, the in a few days and in the daytime coefficient of variation (cat)
It is respectively smaller than 5.41% and 6.03%；In a few days and in the daytime the coefficient of variation (dog) is respectively smaller than 7.29% and 4.63%.
The precision that 3 imidacloprid of table measures in cat blank plasma samples
The precision that 4 imidacloprid of table measures in dog blank plasma samples
To sum up test result, present invention provide that blood plasma in imidacloprid extraction and purification method and selected chromatographic condition
Meet quality assurance of drug, quantitative analysis requirement.
Example of the present invention is the description of the invention and cannot limit the present invention, with the comparable meaning of the present invention
Any change and adjustment in range, are all considered as within the scope of the invention.
Claims (6)
1. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma, includes the following steps:
1) dog or cat plasma sample pre-treatment:
Acetonitrile is added to dog, cat plasma sample, is centrifuged after mixing；It takes supernatant to be dried with nitrogen in 40 DEG C of sand-baths, obtains residue；
Mobile phase solution is added in residue, redissolves, centrifugation, takes supernatant, filtrate is obtained by filtration；
2) high performance liquid chromatography detection:
Chromatographic column: Symmetry C18；Detector: UV detector；Column temperature: 35 DEG C；Detection wavelength: 270 nm；Sample flow
Speed: 1 mL/min；Mobile phase: acetonitrile: ultrapure water；In mobile phase, acetonitrile, ultrapure water volume ratio are 26:74.
2. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma according to claim 1, which is characterized in that
Step 1) specifically: 200 μ L of dog or cat plasma sample is taken, is placed in 2 mL EP pipes, 1 mL of acetonitrile → vortex, 3 min is added,
Ultrasound 3 min, 4 DEG C of 12,000 10 min of r/min centrifugation → supernatant is drawn in 10 mL EP pipes with pipettor, in 40 DEG C
Be dried with nitrogen in sand-bath → 200 μ L of mobile phase solution is added in residue, 3 min of vortex oscillation → by the solution after redissolution moves to 1.5
In mL EP pipe, it being centrifuged 4 DEG C of 10 min, 12000 r/min → take supernatant 0.22 μm of organic membrane filtration and bottled →
Filtrate is analyzed for HPLC.
3. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma according to claim 1, which is characterized in that
The chromatographic peak retention time of imidacloprid standard items is 7.9 min, and the chromatographic peak retention time of dog or cat plasma sample is 7.7
min。
4. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma according to claim 1, which is characterized in that
The liquid chromatograph used are as follows: the 2695 reciprocating pumps in series of constant current mode double plunger of high performance liquid chromatograph Waters.
5. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma according to claim 1, which is characterized in that
Chromatographic column: Symmetry C18 250 mm × 4.6 mm, 5 μm；Detector: 2998 diode of UV detector Waters
Array detector, 3 work station of Empower；Sample volume: 10 μ L.
6. imidacloprid high-efficiency liquid chromatography method for detecting in a kind of dog cat blood plasma according to claim 1, which is characterized in that
Mobile phase solution is the mixture of acetonitrile, ultrapure water in step 1), and in mobile phase solution, acetonitrile, ultrapure water volume ratio are 26:
74。
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