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Method for determining sesamol in essences and flavors through liquid chromatography-tandem mass spectrometry

A flavor and fragrance, tandem mass spectrometry technology, applied in the field of chemical detection, can solve the problems of high performance liquid chromatography, such as poor sensitivity, cumbersome pretreatment steps, and long detection time, and achieve the effects of short detection time, simple operation, and high sensitivity

Active Publication Date: 2014-02-05
CHINA TOBACCO FUJIAN IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these methods have problems such as cumbersome pre-processing steps and long detection time.
For example, there is a problem of long detection time with gas chromatography-mass spectrometry (GC-MS), and it takes more than 40 minutes to detect a sample, and the sensitivity of high-performance liquid chromatography (HPLC) is poor, and the detection limit (LOD) ≥ 80ng / mL, and the required sample volume is large (≥1g)

Method used

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  • Method for determining sesamol in essences and flavors through liquid chromatography-tandem mass spectrometry
  • Method for determining sesamol in essences and flavors through liquid chromatography-tandem mass spectrometry
  • Method for determining sesamol in essences and flavors through liquid chromatography-tandem mass spectrometry

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Experimental program
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Effect test

Embodiment 1

[0046] The present embodiment detects the content of sesamol in the essence and fragrance of tobacco, and the detection method is as follows, and the flow chart of the detection method is as follows: figure 1 shown.

[0047](1) Weigh 0.1g of sesamol (analytically pure), accurate to 0.0001g, dissolve it in methanol, transfer it to a 1000mL volumetric flask, and set the volume to be the standard stock solution; pipette 0.01mL, 0.05mL, 0.1mL respectively mL, 0.5mL, 1.0mL standard stock solution into a 100mL volumetric flask, dilute to volume with 10% (v / v) methanol aqueous solution, then the concentration of sesamol is 0.01μg / mL, 0.05μg / mL, 0.1μg / mL , 0.5 μg / mL, 1.0 μg / mL. Store the standard solution in the dark at 4°C, store it at room temperature when taking it, and use it after reaching room temperature. Make markings once a week;

[0048] (2) Preparation of the sample solution: Weigh about 0.1g of the tobacco flavor and fragrance sample to be tested and place it in a 25mL ...

Embodiment 2

[0063] In this embodiment, the repeatability and standard addition recovery of the method of the present invention are tested, and the detection method is as follows.

[0064] The recovery rate of the method of the present invention was determined by the standard addition method. Weigh 0.1g of the flavor and fragrance sample for tobacco to be tested (the sample is the same as the flavor and fragrance sample used in step (2) of Example 1), and add 0.001mL, 0.005mL, and 0.01mL of Example 1 to each three parts. Sesamol standard stock solution prepared in step (1), and then prepare the spiked sample solution according to the preparation method in Example 1, step (2) "Preparation of sample solution", each sample was measured 6 times, chromatographic and mass spectrometric analysis The condition is the same as embodiment 1, calculates the standard addition recovery rate of sesamol in the flavor and fragrance for tobacco of this method according to analysis result, and the result is ...

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Abstract

The invention relates to a method for detecting sesamol in essences and flavors. According to the method, liquid chromatography-tandem mass spectrometry is adopted for determination, and an external standard method is adopted for quantification. The method has the advantages of short detection time, simplicity and convenience in operation, high sensitivity, high recovery rate, high repeatability and the like. Under the chromatographic conditions of the method, the chromatographic peak of the sesamol is well separated from the chromatographic peak of impurities. The method has a good linear range, the detection limit is 0.002 microgram / mL, the recovery rate is between 90.8 percent and 102.5 percent, the relative standard deviation (RSD) is smaller than 5 percent, and n is equal to 6.

Description

technical field [0001] The invention belongs to the technical field of chemical detection and relates to a method for determining sesamol, in particular to a method for rapidly determining sesamol in flavors and fragrances by means of liquid chromatography-tandem mass spectrometry. Background technique [0002] Today's food safety issues are increasingly concerned by society. The safety of tobacco additives, especially flavor and fragrance additives, has also attracted more and more attention. [0003] Sesamol, also known as 3,4-methylenedioxyphenol, has a very strong antioxidant capacity and is an antioxidant commonly used in the fields of food, medicine, and flavors and fragrances. However, with the advancement of science and technology, the carcinogenic activity of sesamol has gradually been recognized. Toxicology tests have found that sesamol is toxic to the glandular stomach of animals and can cause tumors or cancer in the glandular stomach. In 2006, Japan listed sesa...

Claims

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Application Information

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IPC IPC(8): G01N30/88
Inventor 邓其馨黄朝章苏明亮刘江生刘秀彩黄惠贞蔡国华林艳梁晖谢卫刘泽春
Owner CHINA TOBACCO FUJIAN IND
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