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Method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage.

A technology of calcium methyl butyrate and methyl butyric acid, applied in the field of quality analysis of food and health products, can solve the problems of inability to confirm the target compound qualitatively, incompatibility between the phosphate mobile phase system and mass spectrometry, affecting the confirmation and judgment, etc. Simple sample preparation, high recovery and accuracy, good chromatographic retention and linearity

Inactive Publication Date: 2019-12-27
TAIZHOU VOCATIONAL COLLEGE OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the simple HPLC-UV detection method is a non-confirmative detection method, it cannot be qualitatively confirmed the target compound, which in turn affects the confirmation of whether the sample test result contains β-hydroxy-β-methylbutyric acid
The present invention aims to establish a high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) assay and confirmation method for β-hydroxy-β-methylbutyric acid and its calcium salt in liquid beverages, considering the existing soybean The phosphate mobile phase system in the HPLC-UV method used in the detection of peptide protein powder samples is not compatible with mass spectrometry, and the detection of β-hydroxy-β-methylbutyric acid and its calcium salt in liquid beverages has not been reported. The present invention establishes a high-performance liquid chromatography-tandem mass spectrometry of β-hydroxy-β-methylbutyric acid and its calcium salt in liquid beverages by optimizing the type of chromatographic column, the mobile phase compatible with mass spectrometry, and the sample pretreatment method, etc. (HPLC-MS / MS) determination and confirmation method

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  • Method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage.
  • Method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage.
  • Method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage.

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Embodiment Construction

[0031] The method of the present invention will be described below through specific examples, but the present invention is not limited thereto.

[0032] A method for measuring and confirming beta-hydroxy-beta-methylbutyric acid and its calcium salt in a liquid beverage provided by the present invention is characterized in that the method comprises the following steps:

[0033] 1. Sample pretreatment method

[0034] 1. Pretreatment of liquid beverage samples

[0035] 1.1 Treatment of liquid beverage samples without carbon dioxide: Weigh 1-5g of a uniform sample into a 50mL volumetric flask, add about 25mL of 0.1% formic acid methanol solution, mix well, ultrasonically extract for 10min, cool to room temperature and use 0.1% formic acid methanol solution Dilute to volume and mix well. Transfer an appropriate amount of liquid in the volumetric flask to a plastic centrifuge tube, centrifuge at a speed of ≥10,000 rpm for 5 minutes, and transfer the supernatant to a sample bottle ...

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Abstract

The invention discloses a method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage. The method comprises the following steps of determining and confirming beta-hydroxy-beta-methylbutyric acid in the liquid beverage by adopting high-performance liquid chromatography-tandem mass spectrometry; and converting to obtain the content of the beta-hydroxy-beta-methylbutyric acid calcium salt in the liquid beverage through a conversion coefficient and the determined beta-hydroxy-beta-methylbutyric acid content. The method comprises a sample pretreatment step of determining the beta-hydroxy-beta-methylbutyric acid in the liquid beverage, a blank test method, a determining and confirming step of the high-performance liquid chromatography-tandem mass spectrometry, and a conversion method of the beta-hydroxy-beta-methylbutyric acid calcium salt in the liquid beverage. The method for determining and confirming beta-hydroxy-beta-methylbutyric acid and calcium salt thereof in liquid beverage disclosed by the invention has the advantages of being good in chromatographic retention and linear relation, simple in sample pretreatment and highin recycling rate and accuracy, and can be extensively applied to the quantitative detection and adulteration judgment of the beta-hydroxy-beta-methylbutyric acid and the calcium salt thereof in theliquid beverage sample.

Description

technical field [0001] The invention relates to the field of quality analysis of food and health products, in particular to a method for determining and confirming β-hydroxy-β-methylbutyric acid and its calcium salt in liquid beverages. Background technique [0002] β-Hydroxy-β-methylbutyric acid (CAS: 625-08-1) is a derivative of the essential amino acid leucine produced in vivo through its metabolite α-ketoisocaproic acid. The essential amino acid leucine cannot be synthesized in the human body, and is generally taken from the outside world through diet. In addition to being used for protein synthesis, a small amount of leucine in the human body can produce a small amount of β-hydroxyl-β after metabolism -Methylbutyric acid, under normal dietary conditions, the adult human body can generally produce about 200-400mg of β-hydroxy-β-methylbutyric acid per day. Because β-hydroxy-β-methylbutyric acid can increase muscle synthesis, reduce muscle breakdown, reduce fat, increase ...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06G01N30/04G01N30/86
CPCG01N30/02G01N30/04G01N30/06G01N30/72G01N30/8634G01N30/8665G01N2030/042
Inventor 刘萍
Owner TAIZHOU VOCATIONAL COLLEGE OF SCI & TECH