A method for simultaneous detection of multiple drug residues in poultry meat tissue
A detection method and technology for poultry meat, applied in the field of chromatographic analysis, can solve problems such as inconsistent standards and outdated detection methods for drug residues, and achieve the effects of reducing pollution, saving detection time, and reducing equipment investment.
Active Publication Date: 2017-06-16
SICHUAN NEW HOPE ANIMAL HUSBANDRY TECH
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[0009] The purpose of the present invention is to overcome the defects of outdated and non-uniform standards for drug residue detection methods in the prior art, and provide a detection method for multiple drug residues in poultry meat tissue
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[0050] High-performance liquid chromatography-tandem mass spectrometry is used for detection and analysis, and the condition parameters of chromatography-mass spectrometry in the instrument are set as follows:
[0051] Chromatographic working parameters: Chromatographic column: Phenomenex Kinetex (100mm×4.6mm, 2.6μm), column temperature: 35°C, flow rate: 0.3mL / min, injection volume: 5μL, mobile phase: A contains 5mmol / L ammonium acetate 0.1 % formic acid in water, B is methanol; the gradient elution program is shown in Table 1.
[0052] Mass spectrometry working parameters: electrospray ionization mass spectrometryconditions (ESI); positive and negative ion scanning modes; multiple reaction monitoring (MRM) acquisition mode; desolvation temperature: 350°C; drying gas flow rate: 10.0L / min; atomization Gas pressure: 275.8kPa (40.0psi); capillary voltage: 5500V; resolution: MS1, MS2 are Unit. The mass spectrometry acquisition parameters of each compound were obtained by standard...
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The invention discloses a method for detecting drug residues in poultry tissues. The method comprises the following steps of selecting a poultry sample, adding sodium chloride and acetonitrile, shaking out, adding sodium hydroxide solution, and vibrating for 30s to 5min; then, ultrasonic extracting for 10 to 40min, centrifuging, absorbing supernate for standby use, drying other solution by distillation, adding concentrated hydrochloric acid in the residues, adjusting pH to be about 1 to 3; then, adding acetonitrile, vibration extracting, centrifuging solution subjected to acetonitrile vibration extracting, absorbing supernate to merge with the above supernate, concentrating to dry to obtain sample extracting solution residues; adding a matrix solid-phase dispersion agent and 2ml ethyl acetate, swirling for 2min, taking supernatant liquid, drying through nitrogen, then adding 30 percent of methanol solution containing 0.1 percent of methanoic acid, ultrasonic dissolving, filming and injecting the sample; adopting HLPC-MS to carry out gradient elution detection. According to the method provided by the invention, the current standard one-time one-sample one-item is adjusted to one-time one-sample five-items, so that the time consumed for detection is greatly shortened.
Description
technical field [0001] The invention relates to a chromatographic detection method, in particular to a method for detecting drug residues by ultra-high performance liquid chromatography tandem mass spectrometry, and belongs to the field of chromatographic analysis. Background technique [0002] Poultry meat generally refers to chicken, duck, goose, etc. It is famous for its high protein, low fat, and high nutrition, and plays an important role in people's daily life. Most of the poultry meat sold on the market is large-scale breeding. Due to the high density of poultry gathering in the large-scale breeding process, once a poultry gets sick, it will spread quickly and epidemic diseases will appear. Therefore, general farmers will add an appropriate amount of drugs during the breeding process to prevent the emergence of diseases. Correspondingly, there are clear requirements for the type and time of drug use in the national standard. [0003] In order to increase the breeding...
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IPC IPC(8): G01N30/88
Inventor 易锡斌朱正鹏王虎黄晓琴梁玉树汪春霞周丽陈霞何芸芸裘立群
Owner SICHUAN NEW HOPE ANIMAL HUSBANDRY TECH