CN103091390A - Method for rapidly detecting clenbuterol hydrochloride inside animal body - Google Patents
Method for rapidly detecting clenbuterol hydrochloride inside animal body Download PDFInfo
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- CN103091390A CN103091390A CN2013100027828A CN201310002782A CN103091390A CN 103091390 A CN103091390 A CN 103091390A CN 2013100027828 A CN2013100027828 A CN 2013100027828A CN 201310002782 A CN201310002782 A CN 201310002782A CN 103091390 A CN103091390 A CN 103091390A
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- clenobuterol hydrochloride
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Abstract
The invention provides a method for rapidly detecting clenbuterol hydrochloride inside an animal body. The method comprises the steps of: extracting a body hair on the back of an animal, cutting the body hair into the length as required, then, soaking the cut body hair in ethyl ether, and carrying out oscillation cleaning; and taking out the body hair, subjected to oscillation cleaning, on the back of the animal, and putting the body hair into an ionic mobility spectrometer for detection. The method disclosed by the invention realizes the real-time, rapid and online detection of the clenbuterol hydrochloride inside the animal body.
Description
Technical field
The present invention relates to material detection technique field, relate in particular to a kind of method that detects clenobuterol hydrochloride in animal body.
Background technology
Clenobuterol hydrochloride claims again " clenbuterol hydrochloride ", is a kind of antiasthmatic.This medicine is neither veterinary drug, neither feed addictive, but adrenal gland class CNS stimulant.Forbid within Chinese territory using clenobuterol hydrochloride in feed and animal drinking water from September 10 in 2002.
Before domestic animals slaughter, all to detect sampling to living animal, to detect in animal body whether contain clenobuterol hydrochloride.Mainly to detect by butchering front collection animals urine or blood sample to the detection of clenobuterol hydrochloride at present; Detect and can only carry out LC/MS/MS by meat sample (liver, kidney, muscle etc.) after butchering.And no matter animal is meat producing plant on the hoof detection, government, and society, or the consumer is the individual, is all very important.
But, for the sampling before animal slaughtering, defective that there are the following problems:
1. when gathering the animals urine sample, must wait until that animal drains just voluntarily can complete.But the animal excretion time can't artificially be grasped, and is uncertain large, waste time and energy, and sample to be tested also should not long preservation.Simultaneously, some illegal businessman or raisers can control by medicine the excretion behavior of animal.Make the animals urine sampling have difficult.
2. when gathering the animal blood sample, animals abnormal behaviour occurs because being subject to larger stimulation, has harm sample collection personnel's safety factor.
For this reason, also occurred in prior art detect the method for clenobuterol hydrochloride by the mode that gathers the back part of animal chaeta.With respect to urine sampling and the blood sampling of animal, the collection of back part of animal chaeta is simple and easy to get, and is easy to preserve.Simultaneously, in the back part of animal chaeta metabolism of clenobuterol hydrochloride slower, medicament residue concentration is stable than animal tissue.Existing research report as the target organ that the monitoring Clenbuterol uses, can be used as clenobuterol hydrochloride residue detection in animal body with animal hair both at home and abroad.
But, detection for clenobuterol hydrochloride in animal hair, basically be to adopt Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) to detect at present, its method is: with animal hair through alkali or acid hydrolysis, then after Solid phase extraction separation, purifying, concentrated, constant volume, then can carry out LC-MS/MS and analyze.This detection method can't realize real-time, quick, online detection.
Summary of the invention
For this reason, technical matters to be solved by this invention is: provide the method for clenobuterol hydrochloride in a kind of fast detecting animal body, to realize real-time, quick, the online detection of clenobuterol hydrochloride in animal body.
So, the invention provides the method for clenobuterol hydrochloride in a kind of fast detecting animal body, comprising:
Extract the back part of animal chaeta, and it is cut into the length that needs, then put into and soak oscillation cleaning in ether;
Take out the back part of animal chaeta that cleans after swinging, put in ion migration ratio spectrometer and detect.
Concrete, a kind of method of clenobuterol hydrochloride in fast detecting animal body comprises:
Extract back part of animal chaeta 10g, and it is cut into 1cm length, then put in the 10ml ether and soaked oscillation cleaning 1 minute;
1 to 10 milligram of back part of animal chaeta (approximately 4 ~ 40) after take out cleaning, and put it in ion migration ratio spectrometer and detect.
Get 1 to 10 milligram in back part of animal chaeta 10g after described immersion vibration, put in ion migration ratio spectrometer and detect, heating detected material back part of animal chaeta, heating-up temperature is that 210 degree are between 230 degree, after the hair gasification, if contain clenobuterol hydrochloride in detected hair, bring migration tube by the carrier gas in ion migration ratio spectrometer into through ion gun, and generate product ion and surveyed in migration tube;
The Ion Phase of institute's test sample product is compared differentiation to the clenobuterol hydrochloride ion relative mobility of preserving in mobility spectrum and database, and the Identification display result.
Described Identification display result comprises:
If consistent Ion Phase is arranged to mobility spectrum, shows the title of this material clenobuterol hydrochloride; If there is no consistent Ion Phase to mobility spectrum, show and do not contain any known substance.
The method of clenobuterol hydrochloride in a kind of fast detecting animal body of the present invention, by extracting the back part of animal chaeta, and it is cut into the length that needs, then put into and soak oscillation cleaning in ether, back part of animal chaeta after cleaning is at last put into the method that detects in ion migration ratio spectrometer, has realized real-time, quick, the online detection of clenobuterol hydrochloride in animal body.
Further, described ion migration ratio spectrometer has used the method for relative ion mobility, has realized real-time, quick, the online detection of clenobuterol hydrochloride in animal body.
Description of drawings
Fig. 1 is the schematic flow sheet of the described method of the embodiment of the present invention;
Fig. 2 is the 10ppb clenobuterol hydrochloride ion mobility spectrogram in described ion migration ratio spectrometer in embodiments of the present invention;
Fig. 3 is the 1mg ox back section chaeta ion mobility spectrogram in described ion migration ratio spectrometer in embodiments of the present invention;
Fig. 4 is 10ppb clenobuterol hydrochloride and the 1mg ox back section chaeta ion mobility spectrogram comparison diagram in described ion migration ratio spectrometer in embodiments of the present invention.
Embodiment
Below, describe the present invention by reference to the accompanying drawings.
As shown in Figure 1, the present embodiment provides the method for clenobuterol hydrochloride in a kind of fast detecting animal body, comprising:
Extract ox back part of animal chaeta 10g, and it is cut into 1cm left and right length, then put in the 10ml ether and soaked oscillation cleaning 1 minute;
The ox back section chaeta that cleaned after take out cleaning, and put it in ion migration ratio spectrometer and detect.
Get 1 to 10 milligram (approximately 4 ~ 40) in back part of animal chaeta 10g after described immersion vibration, put in ion migration ratio spectrometer and detect, heating detected material back part of animal chaeta, heating-up temperature is that 210 degree are between 230 degree, after the hair gasification, if contain clenobuterol hydrochloride in detected hair, bring migration tube by the carrier gas in ion migration ratio spectrometer into through ion gun, and generate product ion and surveyed in migration tube;
The Ion Phase of institute's test sample product is compared differentiation to the clenobuterol hydrochloride ion relative mobility of preserving in mobility spectrum and database, and the Identification display result.
Wherein, described heating detected material back part of animal chaeta, heating-up temperature is that 210 degree are between 230 degree, at this temperature, the determinand clenobuterol hydrochloride in hair easily gasifies and is easy to and separates out, and can avoid the hair coking and severe contamination equipment simultaneously, after the hair gasification, if contain clenobuterol hydrochloride in detected hair, bring migration tube by carrier gas into through ion gun, and generate product ion and surveyed in migration tube; The Faraday detector detects gas current and amplifies through amplifier, and after transforming via A/D sampling thief digital-to-analogue, exports to data processing unit;
Data processing unit calculates the ion mobility of described sample molecule and the ion mobility of known substance A, and according to
Perhaps
Obtain relative ion mobility, wherein,
For
Relative ion mobility,
Be the ion mobility of the clenobuterol hydrochloride that contains in detected material,
Ion mobility for known substance A;
The ion relative mobility of the clenobuterol hydrochloride preserved in the ion relative mobility of described sample molecule and database is compared differentiation, and the Identification display result.
Described known substance A is water vapour.
Described Identification display result comprises:
If consistent ion mobility spectrometry is arranged, show the title of this material clenobuterol hydrochloride, if there is no consistent ion mobility spectrometry, also show and do not contain any known substance.
Above-mentioned ion migration ratio spectrometer, and detection method in this ion migration ratio spectrometer number be 201110175660.X by the applicant in Chinese patent application, and denomination of invention is to utilize in the method for ion mobility spectrometry recognition material to disclose.
With each parameter adjustment of described ion migration ratio spectrometer such as following table:
| Title | Describe |
| Working temperature | 50 C° |
| The migration gaseous species | Dry air |
| Migration gas humidity (dewpoint temperature) | -50 C° |
| The migration gas flow | 1000ml/s |
| Migration electric field intensity | 300V/cm |
| The injector working method | Pyrolysis absorption |
| The injector working temperature | 230 C° |
| The sample introduction carrier gas flux | 300ml/s |
Get clenobuterol hydrochloride sample aqueous solution 10ppb, by direct injected 4 μ l, measure under positive ion mode, obtain the standard ionomer mobility spectrogram of known substance A clenobuterol hydrochloride as shown in Figure 2 and consist of corresponding spectrum storehouse.
Above-mentioned ox back section chaeta after having cleaned is put in described ion migration ratio spectrometer, measured under positive ion mode, obtain ion mobility spectrogram as shown in Figure 3.
The spectrogram of the clenobuterol hydrochloride in the ion mobility spectrogram that test 1mg ox back section chaeta obtains in described ion migration ratio spectrometer in embodiments of the present invention and spectrum storehouse compares, and obtains collection of illustrative plates comparison diagram as shown in Figure 4.The present embodiment collection of illustrative plates comparison diagram consistent (having the position coincidence of standard spectrogram) illustrates in this ox animal body and contains clenobuterol hydrochloride.Real-time, quick, the online detection of clenobuterol hydrochloride in animal body have been realized.
In sum, the method of clenobuterol hydrochloride in the described a kind of fast detecting animal body of the embodiment of the present invention, by extracting the back part of animal chaeta, and it is cut into the length that needs, then put into and soak oscillation cleaning in ether, back part of animal chaeta after cleaning is at last put into the method that detects in ion migration ratio spectrometer, has realized real-time, quick, the online detection of clenobuterol hydrochloride in animal body.
Further, described ion migration ratio spectrometer has used the method for relative ion mobility, has realized real-time, quick, the online detection of clenobuterol hydrochloride in animal body.
The above is only preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (4)
1. the method for the interior clenobuterol hydrochloride of fast detecting animal body, is characterized in that, comprising:
Extract the back part of animal chaeta, and it is cut into the length that needs, then put into and soak vibration in ether;
Take out the back part of animal chaeta after described immersion is vibrated, put in ion migration ratio spectrometer and detect.
2. method according to claim 1, is characterized in that, comprising:
Extract back part of animal chaeta 10g, and it is cut into 1cm length, then put into and soak vibration 2 minutes in the 10ml ether;
Take out the back part of animal chaeta after described immersion vibration, and put it in ion migration ratio spectrometer and detect.
3. according to claim 1 or claim 2, it is characterized in that, get 1 to 10 milligram in back part of animal chaeta 10g after described immersion vibration, put in ion migration ratio spectrometer and detect, heating detected material back part of animal chaeta, heating-up temperature is that 210 degree are between 230 degree, after the hair gasification, if contain clenobuterol hydrochloride in detected hair, bring migration tube by the carrier gas in ion migration ratio spectrometer into through ion gun, and generate product ion and surveyed in migration tube;
The Ion Phase of institute's test sample product is compared differentiation to the clenobuterol hydrochloride ion relative mobility of preserving in mobility spectrum and database, and the Identification display result.
4. method according to claim 3, is characterized in that, described Identification display result comprises:
If consistent Ion Phase is arranged to mobility spectrum, shows the title of this material clenobuterol hydrochloride; If there is no consistent Ion Phase to mobility spectrum, show and do not contain any known substance.
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| CN2013100027828A CN103091390A (en) | 2013-01-05 | 2013-01-05 | Method for rapidly detecting clenbuterol hydrochloride inside animal body |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103245715A (en) * | 2013-05-17 | 2013-08-14 | 中国农业科学院农业质量标准与检测技术研究所 | Method for detecting clenbuterol hydrochloride in sample in assisted mode based on ion mobility spectrometry |
| CN109187840A (en) * | 2018-11-08 | 2019-01-11 | 南京大学 | The high flux examination analysis method of organic pollutant in a kind of blood |
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| CN101936946A (en) * | 2009-06-30 | 2011-01-05 | 同方威视技术股份有限公司 | Method for detecting melamine in foods or feeds by using ion mobility spectrometry (IMS) technology |
| CN102253112A (en) * | 2011-06-27 | 2011-11-23 | 武汉矽感科技有限公司 | Method for identifying substance by ion mobility spectrum |
| CN102854237A (en) * | 2011-06-30 | 2013-01-02 | 李德和 | On-site intelligent fast real-time detector of residue of beta-adrenalin receptor agonist adopting ion mobility spectrometry |
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2013
- 2013-01-05 CN CN2013100027828A patent/CN103091390A/en active Pending
Patent Citations (3)
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| CN101936946A (en) * | 2009-06-30 | 2011-01-05 | 同方威视技术股份有限公司 | Method for detecting melamine in foods or feeds by using ion mobility spectrometry (IMS) technology |
| CN102253112A (en) * | 2011-06-27 | 2011-11-23 | 武汉矽感科技有限公司 | Method for identifying substance by ion mobility spectrum |
| CN102854237A (en) * | 2011-06-30 | 2013-01-02 | 李德和 | On-site intelligent fast real-time detector of residue of beta-adrenalin receptor agonist adopting ion mobility spectrometry |
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| 赵晶晶等: "盐酸克伦特罗在小鼠毛发与肝肾和肌肉中残留量关系的研究", 《药物分析杂志》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103245715A (en) * | 2013-05-17 | 2013-08-14 | 中国农业科学院农业质量标准与检测技术研究所 | Method for detecting clenbuterol hydrochloride in sample in assisted mode based on ion mobility spectrometry |
| CN109187840A (en) * | 2018-11-08 | 2019-01-11 | 南京大学 | The high flux examination analysis method of organic pollutant in a kind of blood |
| CN109187840B (en) * | 2018-11-08 | 2020-06-09 | 南京大学 | High-throughput screening and analyzing method for organic pollutants in blood |
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Application publication date: 20130508 |