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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 reagent consumption, and achieve low reagent consumption, high extraction efficiency and high recovery rate Effect

Active Publication Date: 2013-12-25
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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Effect test

Embodiment 1

[0082] The animal source food sample described in this example is a pork negative sample added with 15 kinds of β-receptor agonist standard products, and the added amount is 20 μg / kg. A method for receptor agonist compounds, such as figure 1 As shown, it specifically includes the following steps:

[0083] a. Pretreatment of the sample, specifically including the following steps:

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

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

[0086] (3) Take 5 mL of the first supernatant, tran...

Embodiment 2

[0111] The animal source food sample described in this embodiment is a pork positive sample, and the method for detecting 15 kinds of β-receptor agonist compounds in animal source food by liquid-mass spectrometry specifically includes the following steps:

[0112] a. Pretreatment of the sample, specifically including the following steps:

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

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

[0115] (3) Take 5 mL of the first supernatant, transfer it to a glass test tube containing 600 mg of adsorbent C18 (with a particle size of 40-60 μm), vortex for 1 min to mix the adsorbent and solution evenly, and then centrifuge at 1500 rpm. Xinde second supernata...

Embodiment 3

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

[0142] a. Pretreatment of the sample, specifically including the following steps:

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

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

[0145] (3) Take 5 mL of the first supernatant, transfer it to a glass test tube containing 250 mg of adsorbent C18 (with a particle size of 40-60 μm), vortex for 1 min to mix the adsorbent and solution evenly, and then centrifuge at 1500 rpm. Xinde sec...

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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 in particular relates to a liquid-mass spectrometry method for rapidly detecting clenbuterol in animal source foods, and an applicable sample pretreatment method. Background technique [0002] β-receptor agonists, also known as β-agonists (β-agonists), are a class of synthetic adrenal receptor agonists, including more than a dozen compounds such as clenbuterol hydrochloride, ractopamine, and salbutamol. Clinically, β-receptor agonist compounds can be used to prevent and treat bronchial asthma and bronchospasm in humans and animals. However, the β-receptor agonist is 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 improve the lean meat rate of food animals, reduce the fat of food animals, Promoting animal growth and shortening the growth period of animals can bring mo...

Claims

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Application Information

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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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