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A method for the rapid quantitative determination of l-carnitine in infant formula milk powder by ultra performance liquid chromatography tandem mass spectrometry

An infant formula and ultra-high performance liquid phase technology, which is applied in the field of rapid quantitative detection of L-carnitine in infant formula milk powder, can solve the problems of complex chromogenic solution configuration, high detection limit, poor repeatability of test results, etc. Achieve the effect of avoiding target loss, fast analysis and high sensitivity

Active Publication Date: 2019-12-03
HEBEI SANYUAN FOOD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the national standard for the detection of L-carnitine in infant formula milk powder is GB29989-2013 [6] , spectrophotometer method, but due to the complex configuration of the chromogenic solution; the instability of acetyl-CoA and acetylcarnitine transferase, the test results often have poor repeatability and the detection limit is high (0.6mg / 100g)

Method used

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  • A method for the rapid quantitative determination of l-carnitine in infant formula milk powder by ultra performance liquid chromatography tandem mass spectrometry
  • A method for the rapid quantitative determination of l-carnitine in infant formula milk powder by ultra performance liquid chromatography tandem mass spectrometry
  • A method for the rapid quantitative determination of l-carnitine in infant formula milk powder by ultra performance liquid chromatography tandem mass spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1. Optimization of ultrasonic time in sample pretreatment operation

[0051] For the detection of L-carnitine in milk powder, it is necessary to ensure the uniformity of the sample and reduce the contamination of the instrument by the constant target compound in the sample matrix. In the research of the present invention, some representative samples are taken from the original solid samples, mixed thoroughly, divided by quartering, and then the samples are accurately weighed, and hydrochloric acid solution is added for ultrasonic extraction. The optimization of ultrasound time is explored as follows.

[0052] Weigh five parts of the same sample respectively, add hydrochloric acid solution, ultrasonicate for 5min, 10min, 15min, 20min, 25min respectively, and then test, the final extraction results refer to the attached figure 1 , it can be seen that the ultrasonic extraction time is different and the extraction effect is different, but the comprehensive optimiza...

Embodiment 2

[0053] Example 2. Exploration on Final pH Optimization in Sample Pretreatment Operation

[0054] Adjust the pH gradient with sodium hydroxide solution, 3.5, 3.8, 4.0, 4.5, 5.0, 7.0, and test the L-carnitine content on the machine respectively. Only when the pH is 4.5, the protein precipitation is complete, the filtrate is clear, and in LC / The chromatographic peak shape is the best in MS / MS, so the final pH is determined to be 4.5 in the sample pretreatment operation.

Embodiment 3

[0055] Example 3. Optimization of sample dilution factor in sample pretreatment operation

[0056] Due to the high sensitivity of the LC / MS / MS instrument, the sample must be diluted by a certain number of times to make the L-carnitine content in the treatment solution within the optimal linear range of the instrument. And dilution can also reduce the inhibition of the sample matrix, reduce the signal-to-noise ratio of the instrument, and improve the sensitivity. After the test, it is finally selected that after the treatment solution is constant to 100ml, it must pass through a 0.22 μm filter membrane at this time to achieve a better measurement effect; the obtained filtrate is then diluted 5 times with ultrapure water, which is the best.

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Abstract

The invention discloses a method of quickly quantitatively determining L-carnitine in infantile formula milk powder by using ultra-high performance liquid chromatography and tandem mass spectrometry; CORTECS HILIC chromatographic columns are used for separation, methanol and 0.1% formic acid solution is used as a mobile phase, column temperature is 25 DEG C, sample injection quantity is 2 MuL, flow speed is 0.3 ml / min, an electro-spray ion source is used as a mass spectrometry ion source, positive ion scanning mode is utilized, multi-reaction monitoring is used as a scanning method, and quantitative ions are m / z 162.2-103.1. The method is simple to perform, high in sensitivity and good in repeatability and is useful for determining L-carnitine in infantile formula milk powder.

Description

technical field [0001] The invention relates to the technical field of food inspection, in particular to a rapid quantitative inspection method for L-carnitine in formula milk powder for infants and young children. Background technique [0002] L-carnitine (L-Carnitine), the chemical name is 3-carboxy-4-N-trimethyl-aminobutyric acid (3-Hydroxy-4-N-trimethyla minobutyrate), is a widely existing in the human body Amino acid-like, mainly distributed in muscle and heart, its main function is to transport fat into mitochondria, promote fatty acid burning, and provide energy for the body [1-3] , people can not only obtain L-carnitine through food, but also synthesize it in the body [4] , but infants' self-synthetic ability is low, so it must be supplemented in infant food. [0003] The national standard GB10765-2010 "National Food Safety Standard Infant Formula Food" stipulates: L-carnitine is an optional ingredient, and the minimum addition amount is 0.3mg / 100KJ [5] . At pres...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 刘玲君陈历俊何香婷房新平
Owner HEBEI SANYUAN FOOD