Method for determining content of trimethylamine in egg yolk through headspace gas chromatography
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A kind of headspace gas chromatography, technology of trimethylamine
Inactive Publication Date: 2016-07-06
FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES
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The first two measure the total volatile amines, and the error is relatively large; the sensitivity of gas chromatography after organic solvent extraction is low; the picrate colorimetric method is currently the national stand
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Embodiment 1
[0035] 1. detection method of the present invention is specifically as follows:
[0036] (1) Solution preparation
[0037] Preparation of trimethylamine (TMA) standard stock solution: Add 0.1617g of dried trimethylamine hydrochloride standard product and 1mL of concentrated hydrochloric acid solution to a 100mL volumetric flask, dissolve with ultrapure water and dilute to the mark, shake well, and Prepare a 1000 mg / L trimethylamine stock solution.
[0038] TMA standard solution: Pipette 2 mL of 1000 mg / L TMA standard stock solution and dilute to 100 mL with ultrapure water to prepare 20 μg / mL TMA standard solution, and refrigerate at 4°C for later use.
[0039] Standard sample solution: Add 4.95, 4.9, 4.75, 4.5, 2.5 and 0 mL of ultrapure water into a 20 mL headspace bottle, and add 5 mL of 1.17 g / mL potassium hydroxide solution, and seal the cap. Add 0.05, 0.1, 0.25, 0.5, 2.5, and 5 mL of standard working solution of trimethylamine into the microsyringe puncture, and the s...
Embodiment 2 and Embodiment 3
[0057] Add 4mL of ultrapure water into 20mL headspace bottles, peel off the skin, accurately measure 1mL each of egg yolks (yolk sample 1 and egg yolk sample 2) with known trimethylamine content, a total of 5 parts, weigh, seal, and vortex to mix ;Puncture and add 5mL of 1.17g / mL potassium hydroxide solution, and vortex to mix. Place the headspace bottle in an ultrasonic instrument at 30°C for 30 minutes. The results are shown in Table 3, and the other steps of Examples 2 and 3 are the same as in Example 1.
[0058] The above operation was repeated once, and the results obtained are shown in Table 3.
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Abstract
The invention relates to a method for determining the content of trimethylamine in egg yolk by headspace gas chromatography. The determination method is as follows: potassium hydroxide is used as a catalyst, added to the egg yolk liquid, ultrasonically, and under airtight conditions, trimethylamine is hydrolyzed and completely released from the egg yolk tissue; then trimethylamine hydrochloride is used as a standard solution, and the top Blank injection, gas chromatographic analysis. Calculate the content of trimethylamine in the sample according to the standard curve of standard substance concentration and peak area. The invention is superior to common chemical analysis methods, and has the characteristics of short analysis time, simple operation and high accuracy.
Description
technical field [0001] The invention relates to a method for determining trimethylamine content in egg yolk by headspace gas chromatography, which belongs to the field of food. Background technique [0002] Trimethylamine (trimethylamine, TMA), the molecular formula is (CH 3 ) 3 N (Formula 1), is a highly volatile amine with a fishy odor and a boiling point of 2.87°C. Anhydrous is a colorless liquefied gas, soluble in water, ethanol and ether; it is flammable, with a spontaneous ignition point of 190°C, and is a Class I flammable and highly corrosive gas. The relative density is 0.632. TMA has only a slight odor, and when the concentration increases by 2 to 10 times, the odor becomes aggravated, with a strong fishy smell, and the olfactory threshold concentration is lower than that of ammonia, only 0.002mg / L. Because there are unshared electron pairs on the nitrogen atom, TMA can provide the unshared electron pairs to combine with electron pair acceptors, thus showing ba...
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IPC IPC(8): G01N30/16G01N30/06G01N30/86
CPCG01N30/16G01N30/06G01N30/8637
Inventor 王晶武书庚龙城张海军齐广海
Owner FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES