CN105181839A - Method for detecting residual quantity of ivermectin in sheep muscle tissues by using liquid chromatograph/mass spectrometer with doramectin as internal standard substance - Google Patents
Method for detecting residual quantity of ivermectin in sheep muscle tissues by using liquid chromatograph/mass spectrometer with doramectin as internal standard substance Download PDFInfo
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Abstract
The invention discloses a method for detecting the residual quantity of ivermectin in sheep muscle tissues by using a liquid chromatograph/mass spectrometer with doramectin as an internal standard substance. The method comprises the following steps: extracting ivermectin residual in the sheep muscle tissues with acetonitrile as an extraction solvent, adopting an impurity adsorption and solid phase extraction mode, adopting an alkaline alumina column as a solid phase extraction column, introducing acetonitrile, eluting, and collecting all obtained eluate. The method solves the problems of complex extraction and purification processes and high detection limit of traditional detection methods, realizes enrichment and purification of ivermectin residual in the sheep muscle tissues, improves the detection sensitivity, repeatability and accuracy, and is suitable for batch sample detection.
Description
Technical field
The invention belongs to detection of veterinary drugs in food method field, particularly relate to the method that ivermectin residual in sheep musculature is detected.
Background technology
Ivermectin (Ivermectin, referred to as IVM) be a kind of new macrolide antibiotic, the second generation derivant of Avermectin (Avermectins), it is identical with the expelling parasite mechanism of Avermectin, it is all the realization that is used for by strengthening r-aminobutyric acid (GABA), GABA is a kind of inhibitory neurotransmitter, in the main suppression postsynaptic neuronal conduction of brain GABA, the burst size of GABA increases, it is the potential energy raising of normally stopping of postsynaptic cell, nerve is difficult to stimulus delivery to muscle, muscle can not shrink, parasite is benumbed and is purged, it is one of classic anthelmintic in Avermectin family, applied widely in Animal husbandry production.Ivermectin is widely used as antiparasitic and acaricide in farming and animal husbandry, and such medicine has nerve and development toxicity, and the World Health Organization (WHO) is classified as high cytotoxic compound.Because fat-soluble good, metabolism is slow, long-term a large amount of such medicine of non-reasonable employment, can cause high residue in animal body, thus produces tremendous influence to human health.At present, the relevant report that the detection method remained with ivermectin in sheep musculature is research object is relatively less; The domestic method for ivermectin residue detection mainly contains liquid chromatography UV detection method (HPLC-UV), liquid chromatography fluorescence detection (HPLC-FLD) and immune affinity chromatographic technology (IAC) based on high performance liquid chromatography; Enzyme linked immunological (ELISA) etc.
Liquid phase chromatography in the middle of prior art: being use liquid chromatograph to carry out Component seperation, take ultraviolet spectrophotometer as the content that detecting device detects each component.Owing to there is conjugated diolefine structure in ivermectin molecular structure, at 245nm wavelength, there is strong uv absorption at place, there is numerous endogenous material such as lipid, cortin, vitamin, nucleic acid in this SPECTRAL REGION, the sensitivity of UV-detector is too low, high performance liquid chromatography UV detection method (HPLC-UV) is subject to impurity interference, so cannot meet the retention analysis requirement of Avermectin and toxic metabolite thereof in current agricultural product.
Enzyme linked immunosorbent assay in the middle of prior art: utilize based on the specificity of antigen and antibody, reversibility association reaction, colorimetric is relied on to determine the detection method of medicament residue situation, the existing specific enzyme linked immunological kit of part comes into operation at present, but, immunoassay detects has certain blindness, in China market, euzymelinked immunosorbent assay (ELISA) finished product kit is mostly from external import, and the range of application of euzymelinked immunosorbent assay (ELISA) is subject to larger restriction.
Liquid chromatography fluorescence detection in the middle of prior art: be utilize liquid chromatography to be separated compound, then the ultraviolet of compound or fluorescent characteristic is utilized to carry out qualitative, quantitative qualification, particularly liquid chromatography-fluorescence detection (HPLC-FLD), have that selectivity is good, highly sensitive, advantage of lower cost and be easy to the features such as popularization, detection limit can reach 1ppb, but this detection method needs to carry out derivatization, complicated operation, be not suitable for carrying out a large amount of practicality and detect.
Liquid chromatography mass detection method in the middle of prior art, adopts quantified by external standard method more.The detection of mass detector is sensitiveer, and many factors can cause the inaccuracy of detection, and these easily cause chromatographic peak area unstable, cause the problems such as quantitatively inaccurate.As GB/T21320-2007 etc., its variation within batch coefficient≤20% interassay coefficient of variation≤30%, makes a variation larger.
In existing ivermectin residue detection purification techniques, liquid-liquid extraction method and the C adopting the saturated normal hexane of acetonitrile more
18the solid phase extraction of post, neutral alumina column and alkali alumina post.The liquid-liquid extraction method of the saturated normal hexane of acetonitrile, ivermectin is slightly soluble in normal hexane, also has the loss of a certain amount of ivermectin going deimpurity while.GB/T21320-2007 has then selected C
18and C
8solid-phase extraction column carries out double purified, and running program complexity is loaded down with trivial details.
Summary of the invention
For the deficiency that prior art exists, the technical matters that the present invention solves is: provide a kind of detection method residual for ivermectin in sheep musculature, by to the optimization of existing pretreatment technology and refinement, obtain good enrichment clean-up effect, mark by adding in doractin, carry out Liquid Chromatography-Tandem Mass Spectrometry detection, improve detection method sensitivity, repeatability and accuracy, be applicable to batch samples and detect.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
Be that internal standard compound uses LC-MS instrument to detect a method for ivermectin residual quantity in sheep musculature with doractin, comprise the steps:
Step one, extraction
Take and shred in fresh sheep musculature 2.0g to the 50mL centrifuge tube of mixing, add 8mL acetonitrile, high-speed homogenization 1min, vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, gets supernatant; Use 8mL acetonitrile wash homogenate cutter head again, cleansing solution vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, gets supernatant; Merge supernatant, obtain extract;
Step 2, Solid-Phase Extraction
In alkali alumina solid-phase extraction column, add anhydrous sodium sulfate 2g, first cross post activation with 10ml acetonitrile, then the extract in step one is crossed post, keep flow velocity at 1 ~ 1.5mL/ minute, then wash post with 3mL acetonitrile, collect whole efflux, nitrogen dries up;
Step 3, sample introduction
Step 2 dries up the residue 1.0mL acetonitrile obtained and dissolves, then adds the doractin interior mark liquid that 50 μ L concentration are 1 μ g/mL, vortex 30s, and after crossing 0.22 μm of filter membrane, upper LC-MS instrument detects;
The preparation of step 4, typical curve
Accurately measure the ivermectin standard working solution of a series of concentration respectively, join blank sheep musculature successively, then by step one to three process, drawing standard curve;
Adopt inner mark method ration, calculate the content of ivermectin in sheep musculature according to the result of step 3 and step 4.
Further, liquid phase chromatogram condition is: C
8post; Mobile phase A: acetonitrile, Mobile phase B: containing the 10mmol/L ammonium acetate solution of 0.1vt% formic acid, by V
a: V
b=90:10 ratio mixes; Flow velocity: 0.2mL/min; Column temperature: 25 DEG C; Sample size: 5 μ L.
The beneficial effect of advantage of the present invention and generation is:
This method adopts doractin as the internal standard compound of ivermectin, eliminates the interference of various factors in detecting, is beneficial to accurate quantitative analysis.This method is according to the molecular structure of ivermectin, physicochemical characteristic and alkali alumina post feature, impurity absorption pattern (acetonitrile dissolving-acetonitrile-collection acetonitrile efflux and acetonitrile liquid) is adopted namely to collect all effluxes, reverse phase absorption principle, alkali alumina solid-phase extraction column is in anhydrous weak polar solvent acetonitrile, by the polarity acting force that surface aluminum atoms center is as stronger in oxygen atom is formed with the heteroatoms of the high negative charge of band, the impurity such as the fat that adsorption selection polarity is stronger, collect all effluxes, thus effectively remove impurity interference, improve enrichment and the purification efficiency of residual ivermectin in sheep musculature.
It is low that the inventive method has detectability, highly sensitive, and the coefficient of variation is low, and measurement result is advantage accurately and reliably, is applicable to the detection that in laboratory, in sheep musculature in enormous quantities, ivermectin is residual.
Accompanying drawing explanation
The chemical structural drawing of Fig. 1 ivermectin (a) and doractin (b).
Fig. 2 is the chromatogram that (sheep musculature is added 20ng/mL ivermectin standard solution sample and marked liquid (1 μ g/mL) with 50 μ L doractins are interior) detects object in embodiments of the invention one.
Fig. 3 is the mass spectrogram of doractin (a) and ivermectin (b).
Fig. 4 is that different ions source desolventizing temperature degree is on the impact of ion adducts form.
Fig. 5 is the typical curve of ivermectin.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein is only for instruction and explanation of the present invention, is not intended to limit the present invention.
main material and reagent:
Syringe-type nuclepore membrane filter (0.22 μm, organic system): Tian Jinjin rises experimental facilities company limited;
Acetonitrile, formic acid and ammonium acetate: chromatographically pure, fisher company of the U.S.;
Anhydrous sodium sulfate: analyze pure, Chemical Reagent Co., Ltd., Sinopharm Group;
Watson pure water: Watson company;
Solid phase extraction column: alkali alumina pillar, sepax company of the U.S.;
Ivermectin standard items: content 99.5%, National Institute for Food and Drugs Control;
Internal standard compound doractin: content 96.0%, German DrEhrenstorferGmbH.
key instrument and equipment:
Agilent 1200-6410 LC-MS instrument (HPLC-MS/MS): Agilent company of the U.S.;
High-speed homogenization machine: high honour instrument company of Community of Jin Tan County city;
KL512 type Nitrogen evaporator: Beijing Kang Lin science and technology limited Company;
Hunan instrument hydro-extractor: Xiang Yi company;
Turbula shaker: HerosBIO, RS-2shaker;
KQ-600DE type ultrasonic cleaning instrument: Kunshan ultrasonic cleaning instrument plant.
embodiment 1 different ions source desolventizing temperature degree is on the impact of ion adducts form
ESI ion gun is soft ionization mode, and ivermectin is usual and H in ESI ion gun
+, Na
+, NH
4 +quasi-molecular ion peak is formed Deng combination, wherein, [M+Na]
+ionic structure is stablized, if carry out second order ms cracking to it, is difficult to obtain fragmention, and H
+, NH
4 +etc. can competitively be combined with target molecule, thus cause [M+Na]
+abundance of ions extremely unstable, so multiselect [M+NH during Mass Spectrometer Method
4]
+for parent ion.
One, liquid chromatography and Mass Spectrometry Conditions
1, liquid phase chromatogram condition
Analytical column: Agilent ZORBAXEclipsePlusC
8post; Mobile phase A: acetonitrile, Mobile phase B: containing the 10mmol/L ammonium acetate solution of 0.1% formic acid (percent by volume); Flow velocity: 0.2mL/min; Column temperature: 25 DEG C; Sample size: 5 μ L.
2, Mass Spectrometry Conditions
Electric spray ion source (ESI), positive ion mode, dynamic multiple-reaction monitoring (DynamicMRM) mode gathers, capillary voltage 4kV, collision gas (N
2) flow velocity 10L/min, nebulizer pressure 30psi.
Two, experimental procedure
Select different ions source desolventizing temperature degree, 150 DEG C, 200 DEG C, 250 DEG C, 300 DEG C and 350 DEG C, use mass spectrographic full scan pattern, sample introduction ivermectin standard solution, ivermectin parent ion adduct form under observation different ions source desolventizing temperature degree, [M+Na] of ivermectin
+parent ion peak is m/z897.5, [M+NH
4]
+parent ion peak is m/z892.5.
Three, result
As shown in Figure 4, Fig. 4 is ivermectin [M+Na] under different ions source desolventizing temperature degree to experimental result
+parent ion peak and [M+NH
4]
+parent ion peak.In figure, horizontal ordinate represents ion gun desolventizing temperature degree, and unit is DEG C, and ordinate represents the intensity of quasi-molecular ions.As seen from Figure 4, when desolventizing temperature degree is lower than 200 DEG C, ion adducts is mainly with [M+NH
4]
+form exists; When desolventizing temperature degree equals 250 DEG C, [M+Na]
+the ratio at peak raises rapidly, is substantially equal to [M+NH
4]
+the half of quasi-molecular ions intensity; When reaching 350 DEG C, ivermectin is substantially with [M+Na]
+the form at peak exists.
the standard curve determination experiment of embodiment 2 ivermectin
One, experimental procedure
(1) preparation of standard solution
1, the preparation of doractin inner mark solution
(1) preparation of standard reserving solution: the doractin standard items acetonitrile accurately taking 10mg dissolves and dilutes, and is mixed with the standard reserving solution of 100 μ g/mL, puts in-20 DEG C of refrigerators and keep in Dark Place.
(2) preparation of standard solution: the standard reserving solution accurately drawing 1mL doractin is in 100mL volumetric flask, and the standard solution both having obtained 1 μ g/mL to scale mixing by dilution in acetonitrile is for subsequent use in 4 DEG C of storages.
2, the preparation of ivermectin standard solution
(1) preparation of standard reserving solution: the ivermectin standard items acetonitrile accurately taking 10mg dissolves and dilutes, and is mixed with the standard reserving solution of 100 μ g/mL, puts in-20 DEG C of refrigerators and keep in Dark Place.
(2) preparation of standard intermediate solution: accurately draw 1mL ivermectin standard reserving solution in 100mL volumetric flask, the standard intermediate solution both having obtained 1 μ g/mL to scale mixing by dilution in acetonitrile is for subsequent use in 4 DEG C of storages.
(3) preparation of series standard working solution: with acetonitrile solution stepwise dilution ivermectin standard intermediate liquid be mixed with concentration not wait ivermectin series standard working solution, concentration gradient is 1ng/mL, 5ng/mL, 20ng/mL, 40ng/mL, 80ng/mL, 250ng/mL, 500ng/mL, matching while using.
(2) extract
Take and shred in flesh tissue 2.0g to the 50mL centrifuge tube of mixing, add 8mL acetonitrile, high-speed homogenization 1min, vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, get supernatant to 50mL centrifuge tube.Separately get a 50mL centrifuge tube and add 8mL acetonitrile, washing homogenate cutter head 10s, smashs residue to pieces with glass bar, vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, merges supernatant, obtain acetonitrile extract, for subsequent use.
(3) Solid-Phase Extraction
Get alkali alumina solid-phase extraction column, specification is 1000mg/6mL, anhydrous sodium sulfate 2g is added in this solid phase extraction column, first in this solid phase extraction column, add 10mL acetonitrile to activate, then the acetonitrile extract in step one is crossed post, keep flow velocity at 1mL/ minute ~ 1.5mL/ minute, clean this centrifuge tube with 3mL acetonitrile again and cross post, collect whole efflux in the centrifuge tube of another drying, dry up with nitrogen in Nitrogen evaporator under 50 DEG C of water bath condition, for subsequent use.
(4) liquid phase chromatogram condition
Analytical column: Agilent ZORBAXEclipsePlusC
8post; Mobile phase A: acetonitrile, Mobile phase B: containing the 10mmol/L ammonium acetate solution of 0.1% formic acid (percent by volume), volume ratio is V
a: V
b=90:10; Flow velocity: 0.2mL/min; Column temperature: 25 DEG C; Sample size: 5 μ L.
(5) Mass Spectrometry Conditions
Electric spray ion source (ESI), positive ion mode, dynamic multiple-reaction monitoring (DynamicMRM) mode gathers, capillary voltage 4kV, collision gas (N
2) flow velocity 10L/min, nebulizer pressure 30psi, desolventizing temperature degree 200 DEG C.The mass spectrometry parameters of ivermectin and doractin is as shown in table 1.
Table 1 multiple-reaction monitoring parent ion, daughter ion, cracked voltage and collision energy
* be quantitative daughter ion
(6) sample detection
In step (three), nitrogen blows and add 1.0mL acetonitrile dissolved residue to dry centrifuge tube, add mark liquid (1 μ g/mL) in 50 μ L doractins, vortex 30s, after crossing 0.22 μm of miillpore filter, filtrate measures for HPLC-MS/MS, then calculates the content of ivermectin in sheep musculature according to typical curve.
(7) mensuration of typical curve
Accurately measure the ivermectin series standard working solution 1mL of step () respectively, join in blank sheep muscle samples successively, by step (two) to (six) process, drawing standard curve.
Two, result
Typical curve is shown in Fig. 5.Ivermectin is within the scope of 1ng/mL-500ng/mL, all present good linear relation, related coefficient all reaches 0.9992, regression equation is Y=0.0709X+0.1819, wherein, Y represents the ratio of the chromatographic peak area of ivermectin feature daughter ion m/z307 and the chromatographic peak area of doractin feature daughter ion m/z593.3, and X represents the mass concentration of ivermectin.
the Method validation of the residues detecton of embodiment 3 ivermectin
By the sensitivity of investigation method, repeatability, recovery index, Method validation is carried out to method of the present invention.
One, sensitivity experiment
Process by embodiment 2 step (two) to (six) and analyze and measure mark-on sheep muscle samples, obtain the baseline noise of mark-on sheep muscle within the scope of ivermectin retention time, according to 3 times of signal to noise ratio (S/N ratio) method computing method detection limits, 10 times of signal to noise ratio (S/N ratio) method computing method quantitative limit.Test findings shows, detecting of the inventive method is limited to 0.3 μ g/kg, is quantitatively limited to 0.5 μ g/kg.The U.S., European Union and China are as shown in table 2 for the limitation that ivermectin is residual in sheep muscle, and the residue limits that the detectability of the method and quantitative limit specify far below the U.S., European Union and China, can complete the detection to medicament residue well.
The limitation that table 2 ivermectin is residual in sheep muscle
Two, accuracy and Precision Experiment
10 μ g/kg, 20 μ g/kg and 40 μ g/kg are respectively with the interpolation concentration of ivermectin in sheep muscle, process by embodiment 2 step (two) to (six) and analyze and measure mark-on sheep muscle samples, each concentration level does 5 parallel experiments, in the daytime repeat 5 times, respectively calculate batch in and batch between recovery of standard addition and the coefficient of variation thereof.Under above-mentioned 3 different interpolation concentration levels, the average recovery rate of each test sample is all between 82%-90%, all 6% is less than with interassay coefficient of variation in batch, as shown in table 3, be better than the requirement of GB GB/T21320-2007 variation within batch coefficient≤20% interassay coefficient of variation≤30%.The method meets relevant criterion requirement as can be seen here, and applicability is good, favorable reproducibility, and accuracy is high, meets residual testing requirement.
Table 3 the method measures the withinday precision day to day precision of ivermectin
the determination experiment that in embodiment 4 sheep muscle samples, ivermectin is residual.
One, experimental procedure
(1) drafting of typical curve is with embodiment 2
(2) random each purchase 1 part of sheep muscle samples in 5 supermarkets, every increment product do two Duplicate Samples, process by embodiment 2 step (two) to (six) and analyze and measure sheep muscle samples, according to the peak area data that instrument provides, retention time is qualitative, inner mark method ration, calculates the content of ivermectin in sheep muscle samples.
Two, result
Sample detection result is as table 4, and all samples does not all detect ivermectin and remains.
Table 4 sample detection result
。
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. be that internal standard compound uses LC-MS instrument to detect a method for ivermectin residual quantity in sheep musculature with doractin, comprise the steps:
Step one, extraction
Take and shred in fresh sheep musculature 2.0g to the 50mL centrifuge tube of mixing, add 8mL acetonitrile, high-speed homogenization 1min, vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, gets supernatant; Use 8mL acetonitrile wash homogenate cutter head again, cleansing solution vortex oscillation 2min, the centrifugal 10min of ultrasonic 5min, 4000r/min, gets supernatant; Merge supernatant, obtain extract;
Step 2, Solid-Phase Extraction
In alkali alumina solid-phase extraction column, add anhydrous sodium sulfate 2g, first cross post activation with 10ml acetonitrile, then the extract in step one is crossed post, keep flow velocity at 1 ~ 1.5mL/ minute, then wash post with 3mL acetonitrile, collect whole efflux, nitrogen dries up;
Step 3, sample introduction
Step 2 dries up the residue 1.0mL acetonitrile obtained and dissolves, then adds the doractin interior mark liquid that 50 μ L concentration are 1 μ g/mL, vortex 30s, and after crossing 0.22 μm of filter membrane, upper LC-MS instrument detects;
The preparation of step 4, typical curve
Accurately measure the ivermectin standard working solution of a series of concentration respectively, join blank sheep musculature successively, then by step one to three process, drawing standard curve;
Adopt inner mark method ration, calculate the content of ivermectin in sheep musculature according to the result of step 3 and step 4.
2. method according to claim 1, is characterized in that, liquid phase chromatogram condition is: C
8post; Mobile phase A: acetonitrile, Mobile phase B: containing the 10mmol/L ammonium acetate solution of 0.1vt% formic acid, V
a: V
b=90:10; Flow velocity: 0.2mL/min; Column temperature: 25 DEG C; Sample size: 5 μ L.
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| CN107290451A (en) * | 2017-06-21 | 2017-10-24 | 广东出入境检验检疫局检验检疫技术中心 | Method based on Mo Naitaier and its metabolite residue amount in high performance liquid chromatography series connection quadrupole rod mass spectroscopy animal tissue |
| CN107315054A (en) * | 2017-06-21 | 2017-11-03 | 广东出入境检验检疫局检验检疫技术中心 | A kind of method of Mo Naitaier and its metabolite residue amount in measure dairy products |
| CN108303305A (en) * | 2017-12-20 | 2018-07-20 | 浙江省食品药品检验研究院 | A kind of left drug extractant for livestock meat and its preparation method and application method |
| CN112326815A (en) * | 2020-10-16 | 2021-02-05 | 丽珠集团新北江制药股份有限公司 | Method for detecting multiple antibiotic residues in tissues of livestock by liquid chromatography-mass spectrometry |
| CN113960236A (en) * | 2021-10-11 | 2022-01-21 | 大连海洋大学 | Method for determining geosmin and dimethyl isoborneol in fish body based on rapid pretreatment technology |
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