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Solid phase micro-extraction device and method for measuring volatile organic acid in tobacco leaf

A volatile organic acid, extraction device technology, applied in measurement devices, instruments, scientific instruments, etc., can solve the problems of low analysis sensitivity, complex processing methods, long analysis time, etc., to achieve short analysis time, avoid complexity, The effect of high analytical sensitivity

Inactive Publication Date: 2012-06-20
GUIZHOU TOBACCO SCI INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is: to solve the problem that the extraction and derivatization steps are carried out step by step in the prior art, the processing method is complicated, the repeatability is poor, the analysis time is long and the analysis sensitivity is not high

Method used

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  • Solid phase micro-extraction device and method for measuring volatile organic acid in tobacco leaf
  • Solid phase micro-extraction device and method for measuring volatile organic acid in tobacco leaf
  • Solid phase micro-extraction device and method for measuring volatile organic acid in tobacco leaf

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Determination of volatile organic acids content in first-cured tobacco leaves:

[0027] The first flue-cured tobacco leaves were dried and pretreated at 40°C for 1 h, crushed and passed through a 40-mesh sieve to obtain tobacco powder, which was dried in a vacuum dryer for 12 h for later use. Weigh 20 mg of the above smoke powder into a headspace vial (23×75 mm), add 2 μL of trans-2-hexenoic acid internal standard, and weigh 0.5 g of anhydrous sodium sulfate at the same time, mix well, pour into the glass Add 15 μL of derivatization reagent N, O-bis(trimethylsilyl)trifluoroacetamide to the inner cannula (6×31 mm), place it in the headspace sample vial, and when it is down 60-80° angle, the top of the glass insert is 40-50 mm from the upper cap of the headspace vial, and seal it with the headspace cap. Use the above-mentioned device to perform simultaneous derivation-headspace solid-phase microextraction with a fully automatic solid-phase microextraction device. The con...

Embodiment 2

[0034] Repeatability and recovery determination:

[0035] The same sample analysis method was used to carry out 5 parallel determinations on the same sample by using the device, and the recovery rate was determined by the linear equation obtained by the standard addition method, and the results are shown in Table 2.

[0036] Table 2 Recovery and repeatability of the method

[0037]

[0038] Note: Relative standard deviation (RSD) measurements are five

[0039]The results show that the recovery rates of the 17 kinds of volatile organic acids in the measured tobacco leaves are in the range of 80%-100%, and the average relative standard deviation of the five measurements is 4.1-11.5%, which shows that the determination results of this method High accuracy.

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Abstract

The invention discloses a solid phase micro-extraction device and a method for measuring volatile organic acids in tobacco leaves. The extraction device comprises a solid phase micro-extraction sample injection needle (1) and a headspace sample bottle (4), wherein a glass inner tube (5) is arranged inside the headspace sample bottle (4), a headspace bottle cover (2) is arranged at the mouth of the headspace sample bottle (4), the solid phase micro-extraction sample injection needle (1) is inserted into the headspace sample bottle (4) through the headspace bottle cover (2), and a solid phase micro-extraction fiber head (30 is mounted at the tip of the solid phase micro-extraction sample injection needle. The measurement method comprises the following steps of: weighing a tobacco leaf sample into and putting in the headspace sample bottle, adding internal standard compounds and anhydrous sodium sulfate, thoroughly mixing, sucking derivatization reagents into the glass inner tube, putting the glass inner tube into the headspace sample bottle, sealing the headspace sample bottle with the headspace bottle cover, and performing full automatic headspace solid phase micro-extraction. Compared with the prior art, the method has a simple treatment process and a high analysis speed, and is economical and practical, convenient to operate and environment-friendly.

Description

technical field [0001] The invention relates to a solid-phase microextraction device and a method for measuring volatile organic acids in tobacco leaves. Background technique [0002] Organic acids in tobacco mainly refer to organic acids other than amino acids. Generally, organic acids are divided into volatile, semi-volatile and non-volatile organic acids according to their volatile performance. Usually, lower fatty acids below C10 and some aromatic acids are liquids, which are commonly referred to as volatile acids. . The content of volatile organic acids in flue-cured tobacco is low, the general content is only 0.5 μg / g-100 μg / g, the content is low or even lower than 0.01 μg / g, but it has a great impact on the sensory quality of tobacco. Such as acetic acid, propionic acid, isobutyric acid, isovaleric acid, etc. The volatile organic acids in the tobacco leaves can adjust the pH value of the smoke, reduce the irritation, and make the taste mellow. Therefore, the analy...

Claims

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Application Information

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IPC IPC(8): G01N30/08G01N30/88
Inventor 向章敏周淑平耿召良蔡凯张婕
Owner GUIZHOU TOBACCO SCI INST
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