Method for testing furosine in dairy products

A determination method and technology for dairy products, which are applied in the field of determination of furosine in dairy products, can solve the problems of large interference, high detection limit and low recovery rate.

Inactive Publication Date: 2015-12-30
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The determination of furosine in reconstituted milk requires multiple processes such as hydrolysis, dry filtration, pre-extraction, and HPLC analysis. This method takes a long time to detect, has high detection limits, large interference, and low recovery.

Method used

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  • Method for testing furosine in dairy products
  • Method for testing furosine in dairy products
  • Method for testing furosine in dairy products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Embodiment 1: a preferred embodiment of detection method of the present invention

[0050] Four samples of raw milk, reconstituted milk, pasteurized milk and ultra-high temperature (UHT) instant sterilized milk were selected for testing. Among them, raw milk is regular milk from healthy dairy animals, which has only been cooled and possibly filtered, but has not been pasteurized, heat treated below pasteurization, cleaned milk or other sterilization treatments; reconstituted milk is condensed milk or X Raw milk blended with whole milk powder and water; pasteurized milk is kept at low temperature for a long time (62°C to 65°C for 30 minutes) or at high temperature for a short time (72°C to 76°C for 15s; or 80°C ℃~85℃, kept for 10~15s); ultra-high temperature (UHT) instant sterilized milk is processed by keeping above 135℃ for several seconds.

[0051] (1) Sample preparation

[0052]Take 2.00mL sample with a pipette gun, put it in a heat-resistant test tube with a seal,...

Embodiment 2

[0107] Embodiment 2: Determination of the lower limit of determination

[0108] In the experiment, 3 times the standard deviation of the blank measurement was used as the lower limit of determination, and 10 times the standard deviation was used as the quantitative detection limit. Three parallel measurements were taken to obtain the average value, and the detection limit LOD of the established HPLC method was obtained.

[0109] According to the experimental results, the lower limit of determination of furosine is 0.01 mg / kg, and the quantitative detection limit is 0.04 mg / kg.

Embodiment 3

[0110] Embodiment 3: the mensuration of recovery rate

[0111] Accurately measure two test samples with known fururine content (2.2mg / kg and 2.7mg / kg), and then add a certain amount of standard samples (0.5mg / kg, 1.0mg / kg, 2.0mg / kg ), calculate the standard addition recovery rate according to the above method, the results are shown in Table 3, and Table 3 is the recovery rate of the furosine assay method.

[0112] From the experimental results, the recovery rate of furosine in milk powder ranges from 93.4% to 108.9%.

[0113] table 3

[0114]

[0115]

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Abstract

The invention provides a method for testing furosine in dairy products. The method comprises the following steps: (1) sample preparation, (2) purification, and (3) liquid chromatography and tandem mass spectrum combination, wherein the sample preparation comprises the following steps: conducting pretreatment, heating at 115 DEG C for hydrolysis for 4 h, cooling, conducting dry filtration, and reserving a filtrate for determination; the purification comprises the following steps: putting 0.10 ml of a supernatant into a nitrogen blowing pipe, blow-drying by using a nitrogen blowing concentrator, enabling the volume to be 1.00 ml through a formic acid-ammonium formate buffer solution, fully and uniformly shaking, and transferring the mixture into a sampling bottle through a 1 mL injector filtering film to be subjected to liquid chromatography and tandem mass spectrum testing. The dairy products capable of being tested by the method comprise lactogenesis, reconstituted milk, pasteurized milk or ultra-temperature instant sterilized milk. According to the method, the pretreatment time is shortened, the recovery rate is greatly improved, the tandem mass spectrum is adopted in testing, and the specificity and the sensitivity are improved.

Description

technical field [0001] The invention belongs to the detection field of food additives, in particular to a method for determining furosine in dairy products. Background technique [0002] The contribution of milk to the nutrition and health of Chinese residents is in a period of rapid growth. By 2004, the per capita milk consumption in the country reached 18.8kg. It has damaged the legitimate rights and interests of consumers and farmers and herdsmen, caused unfair competition in the industry, disturbed the order of the industry, and affected the healthy development of my country's dairy industry. Due to high temperature treatment and long-term dry storage, reconstituted milk has a tight protein structure, which reduces the absorption rate and nutritional content compared with fresh milk. Therefore, in order to protect the legal operation of producers and the legitimate rights and interests of consumers, it is of great significance to distinguish whether reconstituted milk is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 韦晓群谢力易敏英庄林洲董洁陈文锐
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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