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A method for determining free butyric acid in milk/dairy products

A technology for dairy products and butyric acid, applied in the field of food safety, can solve the problems of limiting accuracy and precision, increasing adsorption efficiency and separation, and many interfering substances, and achieving high precision, high accuracy and high extraction efficiency. Effect

Active Publication Date: 2020-03-10
BRIGHT DAIRY & FOOD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the low boiling point of butyric acid, the flavor of raw milk and dairy products is complex, and there are many interfering substances, it is necessary to adjust the extraction conditions such as the type of extraction head, extraction equilibrium conditions, adsorption / desorption time, extraction temperature, salt (sodium chloride) concentration, and Chromatography-mass spectrometry and other separation conditions are optimized to increase the adsorption efficiency of the extraction head for butyric acid and the resolution of the instrument; and SPME-GC / MS generally uses the peak area normalization method for semi-quantitative, and the data obtained are only the target compound The percentage of all flavor substances is a proportional data
These detection and quantification methods all limit the accuracy and precision of existing methods

Method used

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  • A method for determining free butyric acid in milk/dairy products
  • A method for determining free butyric acid in milk/dairy products
  • A method for determining free butyric acid in milk/dairy products

Examples

Experimental program
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Effect test

Embodiment 1

[0026] (1) Preparation of standard solution

[0027] Butyric acid standard solution: Accurately weigh 1 g of butyric acid (purity is chromatographic grade) to prepare 1 L of mother liquor and store it in a refrigerator at 4°C for later use. The standard solution is obtained by diluting the mother solution with an appropriate gradient, and it is freshly prepared before use.

[0028] Internal standard solution: Accurately weigh 1 g of heptanoic acid (purity is chromatographic grade), and prepare 1 L of heptanoic acid in ethanol solution with a mass volume ratio of 1 mg / ml, and the concentration of ethanol solution is 5%, and store it in a refrigerator at 4°C for later use.

[0029] (2) Sample processing

[0030] Take 5mL pasteurized milk sample A and place it in a 15mL headspace bottle, add 1.5g sodium chloride and 50μL internal standard solution, and immediately tighten the bottle cap.

[0031] Fatty acid standard sample: Weigh the butyric acid mother liquor to prepare a 55.2...

Embodiment 2

[0045] (1) Preparation of standard solution

[0046] Butyric acid standard solution: Accurately weigh 1 g of butyric acid (purity is chromatographic grade) to prepare 1 L of mother liquor and store it in a 4°C refrigerator for later use. The standard solution is obtained by diluting the mother solution with an appropriate gradient, and it is freshly prepared before use.

[0047] Internal standard solution: Accurately weigh 1 g of heptanoic acid (purity is chromatographic grade), and prepare 1 L of heptanoic acid in ethanol solution with a mass volume ratio of 1 mg / ml, and the concentration of ethanol solution is 5%, and store it in a refrigerator at 4°C for later use.

[0048] (2) Sample processing

[0049] Take 5mL of LUHT sterilized milk sample B and place it in a 15mL headspace bottle, add 2.5g of sodium chloride and 5μL of internal standard solution, and immediately tighten the bottle cap.

[0050] Fatty acid standard sample: Weigh the butyric acid mother liquor to prepa...

Embodiment 3

[0064] (1) Preparation of standard solution

[0065] Butyric acid standard solution: Accurately weigh 1 g of butyric acid (purity is chromatographic grade) to prepare 1 L of mother liquor and store it in a 4°C refrigerator for later use. The standard solution is obtained by diluting the mother solution with an appropriate gradient, and it is freshly prepared before use.

[0066] Internal standard solution: Accurately weigh 1 g of heptanoic acid (purity is chromatographic grade), and prepare 1 L of heptanoic acid in ethanol solution with a mass volume ratio of 1 mg / ml, and the concentration of ethanol solution is 5%, and store it in a refrigerator at 4°C for later use.

[0067] (2) Sample processing

[0068] Take 5mL raw milk sample C and put it in a 15mL headspace bottle, add 0.5g sodium chloride and 50μL internal standard solution, and immediately tighten the bottle cap.

[0069] Fatty acid standard sample: Weigh the butyric acid mother liquor to prepare a 55.2 mg / L standar...

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Abstract

The invention discloses a method for determining free butyric acid in milk / milk products. The method comprises steps as follows: an internal standard substance is added to a to-be-determined substance of the milk / milk products, and the peak area of butyric acid of the to-be-determined substance of the milk / milk products and the peak area of the internal standard substance of the to-be-determined substance of the milk / milk products are obtained with a headspace solid-phase microextraction and gas chromatography-mass spectrometry combined method; an internal standard substance is added to a fatty acid standard sample, and the peak area of butyric acid in the fatty acid standard sample and the peak area of the internal standard substance in the fatty acid standard sample are obtained with the headspace solid-phase microextraction and gas chromatography-mass spectrometry combined method; the content of butyric acid in the to-be-determined substance of the milk / milk products is quantified according to a formula (1). The method for determining free butyric acid in the milk / milk products is simple to operate, high in accuracy, precision and extraction efficiency and applicable to laboratory detection and sample monitoring.

Description

technical field [0001] The invention belongs to the technical field of food safety, in particular to a method for determining free butyric acid in milk / dairy products. Background technique [0002] Free fatty acids in raw milk and dairy products are important compounds that affect their quality, especially the flavor of dairy products. Free fatty acids, as the flavor substances and flavor precursors of milk and dairy products, are generally produced during the processing and manufacturing of dairy products. For example, during the fermentation and maturation of cheese, milk fat will produce free fatty acids under the action of lipase, giving cheese a strong flavor. Characteristic flavor; another example is in liquid milk contaminated by psychrophilic bacteria (especially ultra-high temperature sterilized milk with a long shelf life), fat hydrolysis increases the content of free fatty acids, and eventually causes bad flavors such as fat oxidation and rancidity in the product....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 刘景苏米亚徐致远刘振民
Owner BRIGHT DAIRY & FOOD CO LTD