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Liquid chromatography-mass spectrometry method for rapidly detecting content of beta-agonists and sample pretreatment method

A sample pretreatment and clenbuterol technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of long time consumption and large consumption of reagents, and achieve the effects of small consumption of reagents, high extraction efficiency and simple operation

Active Publication Date: 2015-02-25
BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The problem to be solved by the present invention is that the sample pretreatment method used in the detection of β-receptor agonists in animal source food in the prior art takes a long time and consumes a lot of reagents, and then provides a method suitable for simultaneous and rapid detection of animal Sample pretreatment methods for 15 kinds of β-receptor agonist compounds in food sources, especially for sample pretreatment methods for liquid-mass spectrometry detection;

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  • Liquid chromatography-mass spectrometry method for rapidly detecting content of beta-agonists and sample pretreatment method
  • Liquid chromatography-mass spectrometry method for rapidly detecting content of beta-agonists and sample pretreatment method
  • Liquid chromatography-mass spectrometry method for rapidly detecting content of beta-agonists and sample pretreatment method

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Embodiment 1

[0082] The animal-derived food sample in this example is a pork-negative sample added with 15 kinds of β-receptor agonist standard products, and the addition amount is 20 μg / kg. The liquid-mass spectrometry detects 15 kinds of β-in animal-derived foods. Methods of receptor agonist compounds, such as figure 1 As shown, it specifically includes the following steps:

[0083] a. Pre-treatment of samples, including the following steps:

[0084] (1) Weigh 3g of pork negative sample, add 15 kinds of β-receptor agonist mixed working solution to the sample, control the spiked amount to 20μg / kg, vortex and mix, leave it for about 30min, then add 5mL water, Vortex for 30 seconds, add 10 mL of 1% acetic acid-acetonitrile extraction solution, and extract for 10 minutes under ultrasonic waves of 40 kHz to obtain a mixed solution;

[0085] (2) Add 3g of anhydrous MgSO to the mixed solution 4 And 0.5g NaCl, vortex for 1 minute, and then centrifuge the first supernatant on a centrifuge at 7000 rpm; ...

Embodiment 2

[0111] The animal-derived food sample in this embodiment is a pork positive sample. The liquid-mass spectrometry method for detecting 15 β-receptor agonist compounds in animal-derived food specifically includes the following steps:

[0112] a. Pre-treatment of samples, including the following steps:

[0113] (1) Weigh 3g of positive pork samples, add 3mL of water, vortex for 30s, add 10mL of 1% acetic acid-acetonitrile extraction solution, and extract for 10 minutes under 40kHz ultrasonic to obtain a mixed solution;

[0114] (2) Add 1gMgSO to the mixed solution 4 And 3gNaCl, vortex for 1 minute, and then centrifuge the first supernatant on a centrifuge at 7000rpm;

[0115] (3) Take 5 mL of the first supernatant and transfer it to a glass test tube containing 600 mg of adsorbent C18 (particle size 40-60 μm), vortex for 1 min to mix the adsorbent and the solution uniformly, and then perform separation at 1500 rpm The second supernatant of experience;

[0116] (4) Take 4 mL of the second ...

Embodiment 3

[0141] The animal-derived food in this embodiment is a beef positive sample. The method for detecting 15 β-receptor agonist compounds in animal-derived food by liquid-mass spectrometry specifically includes the following steps:

[0142] a. Pre-treatment of samples, including the following steps:

[0143] (1) Weigh 3g of beef positive sample, add 9mL of water, vortex for 30s, add 15mL of 1% acetic acid-acetonitrile extract, and extract for 10 minutes under 40kHz ultrasonic to obtain a mixed solution;

[0144] (2) Add 6g of anhydrous MgSO to the mixed solution 4 And 1.5g NaAc, vortex for 1 minute, and then centrifuge the first supernatant on a centrifuge at 7000 rpm;

[0145] (3) Take 5 mL of the first supernatant and transfer it to a glass test tube containing 250 mg of adsorbent C18 (particle size 40-60 μm), vortex for 1 min to mix the adsorbent and the solution uniformly, and then perform separation at 1500 rpm The second supernatant of experience;

[0146] (4) Take 4 mL of the second...

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Abstract

The invention provides a liquid chromatography-mass spectrometry method for rapidly detecting the content of beta-agonists. The liquid chromatography-mass spectrometry method comprises the following steps: pretreating a sample, namely, sequentially adding water and an organic extracting solution in the sample for extracting a beta-receptor stimulant; then adding a salting-out agent and a water removing agent to ensure that the organic extracting solution and a water phase demix, centrifuging to obtain a first supernate, adding an adsorbing agent in the first supernate for purification, centrifuging to obtain a second supernate, concentrating, re-dissolving and filtering the second supernate to prepare a sample to be detected; and then detecting the beta-receptor stimulant contained in an animal-derived food by adopting an ultra-high performance liquid chromatography-triple quadrupole mass spectrometer. According to the sample pretreatment method suitable for liquid chromatography-mass spectrometry detection, provided by the invention, interfering molecules are removed through extraction and purification so that high accuracy is achieved in sample detection.

Description

Technical field [0001] The invention belongs to the field of food additive detection, and specifically relates to a method for rapid detection of clenbuterol in animal-derived food by liquid-mass spectrometry, and a suitable sample pretreatment method. Background technique [0002] β-receptor agonists, also known as β-agonists, are a class of synthetic adrenal receptor agonists, including more than a dozen compounds such as clenbuterol, ractopamine, and salbutamol. In clinical medicine, β-receptor agonist compounds can be used to prevent and treat bronchial asthma and bronchospasm in humans and animals. However, β-receptor agonists are also an anabolic agent, which can reduce the synthesis of carcass fat while promoting protein synthesis, so that after being used as a feed additive, it can effectively increase the lean meat rate and reduce the fat of edible animals. Promote the growth of animals and shorten the growth period of animals, which can bring more economic benefits, so...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/08G01N30/14G01N30/02
Inventor 严华张朝晖刘鑫李建辉云环崔凤云
Owner BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU INSPECTION & QUARANTINE TECH CENT
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