CN102778525A - Detection method for residual quantity of salicylanilide veterinary drugs in animal-derived food - Google Patents
Detection method for residual quantity of salicylanilide veterinary drugs in animal-derived food Download PDFInfo
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Abstract
The invention relates to the fields of analytical chemistry and food safety and provides a detection method for residual quantity of salicylanilide veterinary drugs in animal-derived food. According to the detection method, a sample is extracted by using acetonitrile, an obtained extract is purified by using a neutral alumina chromatography column, and then high performance liquid chromatography is utilized to separate and detect two salicylanilide veterinary drugs, wherein 5C18-AR-II is used as a chromatographic column, an aqueous solution system of methanol and 0.1% formic acid is used as a mobile phase and an ultraviolet detector is employed for detection. According to the invention, in a concentration range of 0.03 mu g/mL to 2.5 mu g/mL, good linear relation between content (X) and a peak area (Y) of closantel and rafoxanide is obtained; lower limits of detection of closantel and rafoxanide are both 10 mu g/kg, an average recovery rate of closantel is 73.4 to 84.2%, and an average recovery rate of rafoxanide is 72.9 to 82.6%; coefficients of variation (CV%) of closantel and rafoxanide are 6.7 to 14.7% and 5.7 to 19.8%, respectively; technical indexes like thedetection limit, the recovery rate and precision of the method meet relevant requirements for detection of residual quantity of the veterinary drugs consisting of closantel and rafoxanide at home and abroad.
Description
Technical field
The present invention relates to analytical chemistry, food security field, specifically, is the detection method of salicylanilide class residue of veterinary drug amount in a kind of animal-derived food, relates in particular to the high-efficiency liquid chromatography method for detecting of closantel and two kinds of residue of veterinary drug amounts of rafoxanide kind.
Background technology
Salicylanilide class (Salicylanilides) veterinary drug comprises closantel (Closantel) and rafoxanide (Rafoxanide), is broad-spectrum antiseptic and be one type of broad-spectrum de-worming medicine.Because of its height of tiring, cheap, at home and abroad be used widely in the animal husbandry, become the important drugs of livestock and poultry disease control and prevention.Closantel pair contacts with blood circulation closely or parasitic some nematodes and the Jie Zhi insect of sucking blood property; Like adult and the larva of Fasciola hepatica, fasciola gigantica and great film fluke, haemonchus, Bunostomum trigonoce phalum, intestines and stomach nematode, esophageal orifice nematode, Geiger belong to nematode, Xia Baite nematode etc. all to have and efficiently kills effect.Rafoxanide is ruminated beastly Fasciola hepatica, fascioliasis and haemonchus to treatment ox, sheep etc. and is had very high desinsection effectiveness.
Along with the widespread use and the research of salicylanilide class veterinary drug, find that it has toxicity, side effect.Experiment proof closantel can cause damage to liver, kidney when heavy dose is used.Rafoxanide and protein binding rate are higher, and the half life period is longer, can the residual long period in tissue.Explain that this medicine possibly bring harmful effect to the growing of animal and embryo and fetus of becoming pregnant.Simultaneously, animal foods such as its meat, egg, breast also can produce remote effect to the people.This makes salicylanilide class veterinary drug residual in animal-derived food cause very big attention.
At present, the detection method of salicylanilide class residue of veterinary drug amount mainly contains methods such as microbial method, immunoassay, high performance liquid chromatography, capillary electrophoresis and LC-MS technology.SN/T1628-2005 " importing and exporting closantel determination of residual amount method high performance liquid chromatography in meat and the meat products " discloses closantel determination of residual amount method in meat and the meat products; SN/T1987-2007 " importing and exporting the detection method high performance liquid chromatography of rafoxanide residual quantity in the animal derived food " discloses the detection method of rafoxanide residual quantity in the animal derived food; Stoev G etc. use closantel residual quantity in HPLC-fluorescence detection quantitative measurement tissue, the cow's milk.Sample extracts with acetonitrile, C18 solid-phase extraction column extracting and purifying, and lowest detection is limited to 10 μ g/kg.High performance liquid chromatography such as Zhao Ying are measured closantel sodium content in the preparation.H.A.Benchaoui etc. use high-efficient liquid phase technique and measure closantel and rafoxanide residual quantity in the sheep blood.
Above-mentioned relating in the animal-derived food in the salicylanilide class residue of veterinary drug quantity measuring method, all be only limited to the detection of single residue of veterinary drug amount, and pre-treating method is loaded down with trivial details.The present invention is intended to utilize the high performance liquid chromatography detection technique, sets up a kind of detection method that can detect closantel and rafoxanide residual quantity in the animal-derived food simultaneously.
Summary of the invention
The objective of the invention is to overcome existing not enough problem; Provide a kind of high performance liquid chromatography to detect the method for closantel and rafoxanide residual quantity in the animal-derived food, can make things convenient for, detect simultaneously accurately and efficiently closantel and two kinds of residue of veterinary drug amounts of rafoxanide in the animal-derived food.
The present invention for realizing the technical scheme that above-mentioned purpose adopted is: the detection method of salicylanilide class residue of veterinary drug amount in a kind of animal-derived food may further comprise the steps:
1, sample extraction
2, SPE column purification
Said extracted liquid is crossed the SPE decontaminating column, add 5 mL acetonitriles again when treating liquid level near decontaminating column packing layer upper end, flow velocity is about 1 mL/min; Collect all effluent in the heart bottle; Add 5 mL n-propanols, 40 ℃ down rotation be concentrated near doing, with the moving phase dissolving and be settled to 1 mL; Cross 0.45 μ m filter membrane, supply high-performance liquid chromatogram determination.
3, high performance liquid chromatograph is measured
According to the content situation of closantel in the sample and rafoxanide, the selected close standard operation solution of peak area injects appearance to standard operation solution and appearance liquid equal-volume ginseng, the response of closantel and rafoxanide in metric works solution and the appearance liquid.Qualitative according to the chromatographic peak retention time, adopt the typical curve standard measure.
As preferably, be acetonitrile in the agent of sample extraction described in the step 1.
As preferably, be the neutral alumina decontaminating column at the decontaminating column of SPE described in the step 2, specification 100 * 10 mm (i.d.) load neutral alumina 2 g, warp 10 mL acetonitrile activation before using.
As preferably, at the collocation method of standard solution described in the step 3 be: when disposing single standard reserving solution, closantel is selected acetonitrile-methanol solution system for use, and (9:1 V/V) is solvent, and it is solvent that rafoxanide is selected acetonitrile for use.During configuration hybrid standard storing solution, selecting acetonitrile for use is solvent.
As preferably, be in the condition of liquid-phase chromatographic analysis described in the step 3:
A) chromatographic column: Cosmosil 5C18-AR-II (250 mm * 4.6 mm, 5 μ m)
B) moving phase: methyl alcohol-0.1% aqueous formic acid (93.5:6.5, v/v).
C) flow velocity: 1.0 mL/min
D) column temperature: 35 ℃
E) sample size: 50 μ L
F) detect wavelength: 282 nm
Further, said animal-derived food is selected from beef, beef liver, ox kidney.
Further, said salicylanilide class veterinary drug comprises that closantel and rafoxanide are at least a.
Because adopt technique scheme, beneficial effect of the present invention is:
1, set up the high-efficiency liquid chromatography method for detecting of middle closantel of animal tissue's (muscle, liver, kidney) and rafoxanide residue of veterinary drug amount.Detect when having realized two kinds of salicylanilide class veterinary drugs.
2, animal tissue, liver, kidney etc. are rich in the samples using acetonitrile removal protein of protein, in conjunction with the extraction of homogeneous method, low-temperature and high-speed centrifuging, extraction efficiency is high, and the impurity stripping is few in the extract.
3, extract adopts the neutral alumina decontaminating column to purify, and through the optimization to purification condition, has clean-up effect preferably, and guarantees that two kinds of salicylanilide class veterinary drugs all have the higher recovery.
4, with in the past method relatively, have easy, fast, accurately; Advantages such as sensitivity height; The detection lower bound of closantel and rafoxanide is 10 μ g/kg, and average recovery rate is respectively: closantel 73.4～84.2%, rafoxanide 72.9～82.6%.The coefficient of variation (CV%) is respectively: closantel 6.7～14.7%, rafoxanide 5.7～19.8%.The detection lower bound of method satisfies the requirement of domestic and international relevant laws and regulations, and technical indicators such as precision, the recovery meet the regulation of relevant criterion.
5, the present invention can be applicable in the check of salicylanilide class residue of veterinary drug in the animal product, to promoting the foreign trade of China's animal-derived food, guarantees food security, ensures that human body health all has crucial meaning.
Description of drawings:
Fig. 1 closantel and rafoxanide standard solution high-efficient liquid phase chromatogram; Retention time among the figure (min): closantel 10.965, rafoxanide 14.174;
The blank beef of Fig. 2 adds closantel and rafoxanide standard solution (10 μ g/kg) high-efficient liquid phase chromatogram; Closantel 10.966min among the figure, rafoxanide 14.175min;
The blank beef liver of Fig. 3 adds closantel and rafoxanide standard solution (10 μ g/kg) high-efficient liquid phase chromatogram; Closantel 10.966min among the figure, rafoxanide 14.175min;
The blank ox kidney of Fig. 4 adds closantel and rafoxanide standard solution (10 μ g/kg) high-efficient liquid phase chromatogram; Closantel 10.967min among the figure, rafoxanide 14.175min.
Embodiment:
Below in conjunction with specific embodiment the present invention is done further explain, but the present invention is not limited to specific embodiment.
The detection method of salicylanilide class residue of veterinary drug amount in embodiment 1 beef
1, sample extraction: really take by weighing beef sample 5.0 g that shredded in 100 mL tool cap centrifuge tubes, add 20 mL acetonitriles, behind 10 000 r/min homogeneous, 1 min,, get supernatant with 4 ℃ of 8 000 r/min centrifugal 5 min down.Sediment adds 10 mL acetonitriles again, repeats to extract once, merges supernatant, and is to be clean.
2, SPE column purification: the direct mistake of said extracted liquid is loaded the neutral alumina post of the warp 10 mL acetonitrile activation of 2 g, add 5 mL acetonitriles again when treating liquid level near the alumina layer upper end, flow velocity is about 1 mL/min; Collect all effluent in the heart bottle; Add 5 mL n-propanols, 40 ℃ down rotation be concentrated near doing, with the moving phase dissolving and be settled to 1 mL; Cross 0.45 μ m filter membrane, supply high-performance liquid chromatogram determination.
3, high performance liquid chromatograph is measured: according to the content situation of measured object closantel and rafoxanide in the sample; Choose the close standard operation solution of response and carry out HPLC mensuration together; To standard operation solution and the irregular sample introduction of appearance liquid equal-volume, the response of closantel and rafoxanide all should be in the range of linearity of instrument detecting in metric works solution and the appearance liquid.Qualitative according to the peak retention time, adopt the typical curve standard measure according to peak area.
The liquid-phase chromatographic analysis condition:
Chromatographic column: Cosmosil 5C18-AR-II (250 mm * 4.6 mm, 5 μ m)
Moving phase: methyl alcohol: 0.1% aqueous formic acid=93.5:6.5 (v/v)
Flow velocity: 1.0 mL/min
Column temperature: 35 ℃
Sample size: 50 μ L
Detect wavelength: 282 nm
4, linear relationship test: with the standard reserving solution stepwise dilution; The series mixed standardization working fluid of six variable concentrations of preparation; Concentration range is 0.03 μ g/mL～2.5 μ g/mL, by concentration from low to high, measures according to above-mentioned chromatographic condition and mass spectrum condition.Each concentration determination 3 times is made typical curve with concentration of standard solution Y (μ g/mL) to peak area mean value X (mAU), calculates regression equation and related coefficient.
Closantel typical curve regression equation: Y=57.7572 X+0.045, related coefficient: r=0.99993
The typical curve regression equation of rafoxanide: Y=42.9658 X+ 0.009, related coefficient: r=0.99996
5, the recovery and precision test: accurately take by weighing the beef sample that does not contain chlorocyaniosaliamine amine, rafoxanide, add the closantel and the rafoxanide of 3 different content levels respectively, the interpolation level is seen table 1.Each concentration is carried out 6 parallel sample, analyzes according to above-mentioned chromatographic condition by above-mentioned.The recovery and coefficient of variation result of calculation are seen table 2.
Table 1 recovery and precision test interpolation level (μ g/kg)
| | Level | 1 | | |
| Closantel | 10 | 100 | 500 | |
| Rafoxanide | 10 | 100 | 500 |
Add salicylanilide class veterinary drug Precision test result (n=6) in table 2 beef
Visible by table 2 result: the average recovery rate of three interpolation levels of salicylanilide class medicine is respectively in the beef: closantel 78.2～80.8%, rafoxanide 77.6～80.8%; The coefficient of variation (CV%) is respectively: closantel 9.4～11.1%, rafoxanide 8.6～19.8%.
6, detecting lower bound measures: the blank sample with beef adds test, tries to achieve the detection limit (LOD) of method to 2 kinds of salicylanilide class medicines to be measured with 3 times of signal to noise ratio (S/N ratio)s.Closantel, the rafoxanide detection lower bound in beef sample is 10 μ g/kg.
7, method optimizing process
1. chromatographic column: according to the scope of application of stationary phase in the basic theory, and belong to low pole character and molecular weight ranges, can use C from sample to be analyzed
18The chromatographic column of/ODS filler.Compared L μ na C
18, Eclipse XDB-C
18And 5C
183 kinds of analytical columns of-AR-II, preferred 5C
18-AR-II (250 mm * 4.6 mm, 5 μ m) chromatographic column.
2. moving phase: tested at 5C18-AR-II (250 mm * 4.6 mm; 5 μ m) chromatographic column condition current downflow mutually in the different proportion of methyl alcohol and 0.1 % aqueous formic acid to endogenous impurity disturbed condition in the separating effect of closantel and rafoxanide and the sample, particular methanol: 0.1% aqueous formic acid=93.5:6.5 (v/v)
3. chromatogram column temperature: chromatogram column temperature changes influencing greatly separating of closantel and rafoxanide.Along with the continuous rising of column temperature, retention time is short more, and it is fast more to go out the peak, and impurity peaks is also more and more obvious.For avoiding the influence of column temperature fluctuation, 35 ℃ of preferred constant chromatogram column temperatures.
4. ultraviolet detection wavelength: the ultra-violet absorption spectrum of the mixed standard solution through measuring closantel and rafoxanide, find that closantel and rafoxanide have peak response at 220 nm places, but also maximum of while matrix interference.Take all factors into consideration UV response value and matrix interference situation, preferred 282 nm wavelength are for detecting wavelength.
5. extract solvent: according to the physicochemical property and the coherent reference data of closantel and rafoxanide; Select acetonitrile as extraction agent; Except that well the extraction effect, reducing the stripping of matrix impurity such as albumen precipitation simultaneously to closantel and rafoxanide.
6. sample purification condition: compared the clean-up effect of C18 column purification florisil silica, aluminium oxide decontaminating column, the result show the sample that purifies through alumina column have recovery height, the recovery stable, disturb characteristics such as impurity is few, the easy easy operating of method.
The detection method of salicylanilide class residue of veterinary drug amount in embodiment 2 beef livers
1, sample extraction: really take by weighing beef liver sample 5.0 g that shredded in 100 mL tool cap centrifuge tubes, add 20 mL acetonitriles, behind 10 000 r/min homogeneous, 1 min,, get supernatant with 4 ℃ of 8 000 r/min centrifugal 5 min down.Sediment adds 10 mL acetonitriles again, repeats to extract once, merges supernatant, and is to be clean.
2, SPE column purification: with embodiment 1.
3, high performance liquid chromatograph is measured: with embodiment 1.
4, linear relationship test: with embodiment 1.
5, the recovery and precision test: accurately take by weighing the beef liver sample that does not contain chlorocyaniosaliamine amine, rafoxanide, add the closantel and the rafoxanide of 3 different content levels respectively, the interpolation level is seen table 1.Each concentration is carried out 6 parallel sample, analyzes according to above-mentioned chromatographic condition by above-mentioned.The recovery and coefficient of variation result of calculation are seen table 3.
Add salicylanilide class veterinary drug Precision test result (n=6) in table 3 beef liver
Visible by table 3 result: the average recovery rate of three interpolation levels of salicylanilide class medicine is respectively in the beef liver: closantel 73.4～80.8%, rafoxanide 81.1～82.6%; The coefficient of variation (CV%) is respectively: closantel 6.7～9.5%, rafoxanide 5.7～11.1%.
6, detecting lower bound measures: the blank sample with beef liver adds test, tries to achieve the detection limit (LOD) of method to 2 kinds of salicylanilide class medicines to be measured with 3 times of signal to noise ratio (S/N ratio)s.Closantel, the rafoxanide detection lower bound in beef sample is 10 μ g/kg.
The detection method of salicylanilide class residue of veterinary drug amount in 3 Ns of kidneys of embodiment
1, sample extraction: really take by weighing ox kidney sample 5.0 g that shredded in 100 mL tool cap centrifuge tubes, add 20 mL acetonitriles, behind 10 000 r/min homogeneous, 1 min,, get supernatant with 4 ℃ of 8 000 r/min centrifugal 5 min down.Sediment adds 10 mL acetonitriles again, repeats to extract once, merges supernatant, and is to be clean.
2, SPE column purification: with embodiment 1.
3, high performance liquid chromatograph is measured: with embodiment 1.
4, linear relationship test: with embodiment 1.
5, the recovery and precision test: accurately take by weighing the ox kidney sample that does not contain chlorocyaniosaliamine amine, rafoxanide, add the closantel and the rafoxanide of 3 different content levels respectively, the interpolation level is seen table 1.Each concentration is carried out 6 parallel sample, analyzes according to above-mentioned chromatographic condition by above-mentioned.The recovery and coefficient of variation result of calculation are seen table 4.
[0043] adds salicylanilide class veterinary drug Precision test result (n=6) in the table 4 ox kidney
Visible by table 6 result: the average recovery rate of three interpolation levels of salicylanilide class medicine is respectively in the ox kidney: closantel 79.7～84.2%, rafoxanide 72.9～80.0%; The coefficient of variation (CV%) is respectively: closantel 8.4～14.7%, rafoxanide 10.6～11.7%;
6, detecting lower bound measures: the blank sample with the ox kidney adds test, tries to achieve the detection limit (LOD) of method to 2 kinds of salicylanilide class medicines to be measured with 3 times of signal to noise ratio (S/N ratio)s.Closantel, the rafoxanide detection lower bound in beef sample is 10 μ g/kg.
Claims (7)
1. the detection method of salicylanilide class residue of veterinary drug amount in the animal-derived food is characterized in that this method comprises the steps:
(1) sample extraction
Add 20 mL extraction agents, behind 10 000 r/min homogeneous, 1 min, with 4 ℃ of following centrifugal 5 min of 8 000 r/min, get supernatant, sediment adds 10 mL extraction agents again, repeats to extract once, merges supernatant, and is to be clean;
(2) SPE column purification
Said extracted liquid is crossed the neutral alumina decontaminating column, add 5 mL acetonitriles again when treating liquid level near the alumina layer upper end, flow velocity is about 1 mL/min; Collect all effluent in the heart bottle; Add 5 mL n-propanols, 40 ℃ down rotation be concentrated near doing, with the moving phase dissolving and be settled to 1 mL; Cross 0.45 μ m filter membrane, supply high-performance liquid chromatogram determination;
(3) high performance liquid chromatograph is measured
According to the content situation of closantel in the sample and rafoxanide, the selected close standard operation solution of peak area injects appearance to standard operation solution and appearance liquid equal-volume ginseng, the response of closantel and rafoxanide in metric works solution and the appearance liquid;
Qualitative according to the chromatographic peak retention time, adopt the typical curve standard measure.
2. the detection method of salicylanilide class residue of veterinary drug amount in the animal-derived food in the animal-derived food according to claim 1 is characterized in that the sample extraction agent is an acetonitrile in the step (1).
3. the detection method of salicylanilide class residue of veterinary drug amount in the animal-derived food according to claim 1; It is characterized in that the SPE decontaminating column is the neutral alumina decontaminating column described in the step (2); Specification 100 * 10 mm (i.d.) load neutral alumina 2 g, warp 10 mL acetonitrile activation before using.
4. the detection method of salicylanilide class residue of veterinary drug amount in the animal-derived food according to claim 1; The collocation method that it is characterized in that said standard solution described in the step (3) is: when disposing single standard reserving solution; Closantel is selected acetonitrile-methanol solution system (9:1 for use; V/V) be solvent, it is solvent that rafoxanide is selected acetonitrile for use; During configuration hybrid standard storing solution, selecting acetonitrile for use is solvent.
5. the detection method of salicylanilide class residue of veterinary drug amount in the animal-derived food according to claim 1 is characterized in that the liquid-phase chromatographic analysis condition is described in the step (3):
Chromatographic column: Cosmosil 5C18-AR-II (250 mm * 4.6 mm, 5 μ m)
Moving phase: methyl alcohol-0.1% aqueous formic acid (93.5:6.5, v/v)
Flow velocity: 1.0 mL/min
Column temperature: 35 ℃
Sample size: 50 μ L
Detect wavelength: 282 nm.
6. according to the detection method of salicylanilide class residue of veterinary drug amount in each described animal-derived food in the claim 1 to 5, it is characterized in that said animal-derived food is selected from least a of beef, beef liver, ox kidney.
7. according to the detection method of salicylanilide class class residue of veterinary drug amount in each described animal-derived food in the claim 1 to 5, it is characterized in that said salicylanilide class veterinary drug comprises that closantel and rafoxanide are at least a.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107238668A (en) * | 2017-06-22 | 2017-10-10 | 深圳天祥质量技术服务有限公司 | The detection method of a variety of Residual Veterinary Medicines in animal-derived food |
| CN108593801A (en) * | 2018-05-23 | 2018-09-28 | 湖南农业大学 | A method of measuring pyraclostrobin residual quantity in shaddock using high performance liquid chromatograph |
| CN112763586A (en) * | 2020-11-25 | 2021-05-07 | 华南农业大学 | Chiral chromatographic separation analysis method of closantel enantiomer |
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| WO1993018408A1 (en) * | 1992-03-02 | 1993-09-16 | Enfer Technology Limited | Veterinary drug residue surveillance in fresh meat |
| WO2007046507A1 (en) * | 2005-10-19 | 2007-04-26 | Nippon Meat Packers, Inc. | Extraction liquid for assaying residual veterinary drug |
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| WO1993018408A1 (en) * | 1992-03-02 | 1993-09-16 | Enfer Technology Limited | Veterinary drug residue surveillance in fresh meat |
| WO2007046507A1 (en) * | 2005-10-19 | 2007-04-26 | Nippon Meat Packers, Inc. | Extraction liquid for assaying residual veterinary drug |
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| Title |
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| HOI-SZE YEUNG等: "Screening of closantel and rafoxanide in animal muscles by HPLC with fluorescence detection and confirmation using MS", 《JOURNAL OF SEPARATION SCIENCE》 * |
| 中华人民共和国国家质量监督检验检疫总局发布: "动物源食品中雷复尼特残留量的检测方法 高效液相色谱法", 《中华人民共和国出入境检验检疫行业标准SN/T1987-2007》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107238668A (en) * | 2017-06-22 | 2017-10-10 | 深圳天祥质量技术服务有限公司 | The detection method of a variety of Residual Veterinary Medicines in animal-derived food |
| CN108593801A (en) * | 2018-05-23 | 2018-09-28 | 湖南农业大学 | A method of measuring pyraclostrobin residual quantity in shaddock using high performance liquid chromatograph |
| CN112763586A (en) * | 2020-11-25 | 2021-05-07 | 华南农业大学 | Chiral chromatographic separation analysis method of closantel enantiomer |
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Application publication date: 20121114 |