Method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry

A technology of high performance liquid chromatography and trimethylamine, applied in the field of detection of trimethylamine by high performance liquid chromatography-mass spectrometry, can solve the problems of low detection sensitivity, long detection cycle, poor stability, etc., and achieve high sensitivity and low detection limit , the effect of reducing loss

Inactive Publication Date: 2020-04-28
深圳市农产品质量安全检验检测中心
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to overcome the defects of high detection limit, long detection cycle, low detection sensitivity and poor stability of the detection method of trimethylamine in food in the prior art, and provide a method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry method

Method used

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  • Method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry
  • Method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry
  • Method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] 1. Selection of extractant

[0054] (1) Prepare 10, 20, 50, 100, 200 ng / mL standard solutions of trimethylamine with 5% trichloroacetic acid, 80% acetonitrile and 10% methanol respectively. Perform high-performance liquid chromatography-mass spectrometry detection (consistent detection conditions) and draw a standard curve. The detection result standard curve of the standard solution prepared by 5% trichloroacetic acid is shown in Table 1, figure 1 ; The detection result and standard curve of the standard solution prepared by 80% acetonitrile are as table 2, figure 2 The detection result and standard curve of the standard solution prepared by 10% methanol are as table 3, image 3 .

[0055] Table 1 The detection results of the standard solution prepared by 5% trichloroacetic acid

[0056]

[0057]

[0058] Table 2 The detection results of the standard solution prepared by 80% acetonitrile

[0059]

[0060] Table 3 The detection results of the standard sol...

Embodiment 2

[0074] Example 2 A sample pretreatment method for detecting trimethylamine in food

[0075] (1) Pre-processing:

[0076] Weigh 3g of the sample into a 50mL centrifuge tube, add 6mL of 5% trichloroacetic acid to precipitate the protein, mix it with a mixer for 10min, extract it ultrasonically in an ice bath for 15min, centrifuge at a high speed (6000r / min) for 10min, and transfer the supernatant with a rubber dropper Put it into a 15mL centrifuge tube, and then use 6mL of 5% trichloroacetic acid to repeat the above operation to extract once, combine the two extracts, set the volume to 15mL, centrifuge at a high speed (6000r / min) for 10min, take 5mL of the supernatant and pass it through the PRIME HLB column For purification (no activation required), take 1 mL of the filtrate after passing through the column and pass it through a 0.22 μm membrane for use on the machine.

[0077] (2) Liquid chromatography and mass spectrometry conditions

[0078] Chromatographic conditions

[...

Embodiment 3

[0099] Using the experimental method of Example 2, 32 samples of duck eggs randomly purchased from the Shenzhen farmer's market were measured in parallel, and the average concentration was taken as the content of trimethylamine in the sample. Among them, the measured values ​​in the ultra-linear range were measured on the machine after dilution. The results are shown in Table 10.

[0100] Table 10 Determination of trimethylamine content in duck eggs samples

[0101] Sample serial number YD-1 YD-2 YD-3 YD-4 YD-5 YD-6 YD-7 YD-8 Concentrationμg / kg 1.21×10 5

16.2 20.9 21.8 23.6 31.3 48.0 35.3 Sample serial number YD-9 YD-10 YD-11 YD-12 YD-13 YD-14 YD-15 YD-16 Concentrationμg / kg 22.3 17.9 28.1 23.2 17.4 17.6 22.5 46.3 Sample serial number YD-17 YD-18 YD-19 YD-20 YD-21 YD-22 YD-23 YD-24 Concentrationμg / kg 31.9 37.4 17.0 27.9 28.0 29.7 21.6 30.3 Sample serial number YD...

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Abstract

The invention provides a method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry. The method comprises: S01, adding an extraction agent to a sample to be detected, and carrying out ultrasonic extraction under an ice bath condition; S02, carrying out centrifuging, and separating supernatant and precipitate; S03, adding an extracting agent into the precipitate, and carrying out repeated centrifuging; and S04, combining the supernatant obtained by each centrifugation, carrying out purifying, and carrying out high performance liquid chromatography-mass spectrometry detection. The trimethylamine is detected by utilizing the established method; the content of trimethylamine in an actual sample is converted according to the matrix inhibition ratio of trimethylamine in food. The method is simple to operate, economical and practical; the standard curve of trimethylamine obtained in a range of 0 to 200ng / mL has the linear correlation R being 0.9994, the detection limit being 11.2 microgramme / kg, the low detection limit reaching ppb level, the high sensitivity; and the method can be used for accurately detecting trimethylamine in food.

Description

technical field [0001] The invention relates to the field of analysis and detection, in particular to a method for detecting trimethylamine by high performance liquid chromatography-mass spectrometry. [0002] technical background [0003] Trimethylamine (TMA) is trimethylamine, the molecular formula is C 3 h 9 N, is the simplest tertiary amine, a colorless gas with fish oil odor, soluble in water, ethanol, ether, flammable and poisonous. Trimethylamine in liquid or gaseous state is irritating and corrosive, which can cause skin burns, eye discomfort, respiratory tract irritation, etc., and even death in severe cases. In addition, my country does not have clear regulations on the content of trimethylamine in food, but there have been patients with trimethylaminuria (stinky fish syndrome), who cannot metabolize trimethylamine in their bodies. Trimethylamine mainly exists in poultry eggs, milk, beans, fish, viscera and other foods. The measured value of trimethylamine is oft...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/72G01N30/86
CPCG01N30/02G01N30/06G01N30/7266G01N30/8637G01N2030/062
Inventor 罗燕徐少华吴雯娟丁燕玲黄敏通陈彤钟名琴
Owner 深圳市农产品质量安全检验检测中心
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