Method for detecting aldehydes in rice

A technology for rice and aldehydes, which is applied in the field of analysis and detection of aldehydes, can solve problems such as inaccurate detection results, and achieve the effects of ensuring accuracy, improving authenticity and reliability, and improving the recovery rate of standard addition

Active Publication Date: 2014-12-24
TSINGTAO BREWERY
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Problems solved by technology

[0005] The present invention aims at the problems that aldehydes are easy to be newly produced in the existing detection process, which leads to inaccurate detection results, etc., researches measures to improve the uniformity of aldehydes in rice, measures to reduce the degradation of unsaturated fatty acids to produce aldehydes, etc., and provides A detection method with simple operation and rich detection types, accurate and quantitative detection of 9 kinds of aldehydes in rice by derivatized SPME-GC-MS

Method used

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  • Method for detecting aldehydes in rice
  • Method for detecting aldehydes in rice
  • Method for detecting aldehydes in rice

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] (1) The rice sample was crushed three times through a cyclone mill and passed through a 120-mesh sieve.

[0042] (2) Add the sample to be tested into the headspace bottle, fill the headspace bottle with inert gas argon, cover the bottle cap and place it on the sample tray.

[0043] (3) Headspace derivatized solid-phase microextraction was completed with the help of a multifunctional sampler. Insert the 65 μm PDMS / DVB extraction head into the headspace bottle filled with the derivatization solution o-pentafluorobenzyl hydroxylamine for 20 minutes for derivatization. Then insert the extraction head into the headspace vial containing the rice sample and extract at 40°C for 80 minutes.

[0044] (4) Insert the extraction head into the GC-MS inlet, desorb for 2 minutes and enter the GC-MS detection.

[0045] (5) The chromatographic conditions during detection are: chromatographic column HP-5ms (60m×0.32mm×0.25μm). The carrier gas is helium at a flow rate of 1.5 mL / min. Th...

Embodiment 2

[0049] (1) Effect of water addition on sample detection

[0050] Whether there is water in the detection process has a great influence on the detection of aldehydes. On the one hand, aldehydes may be contained in the water to interfere with the detection of samples. On the other hand, the enzyme activity in aqueous solution is relatively large, such as lipoxygenase, and lipoxygenase will oxidize fatty acids. This produces aldehydes. When detecting aldehydes in water, it is found that the content of acetaldehyde, valeraldehyde and hexanal is high, and acetaldehyde has great interference on the detection of samples (such as figure 1 shown).

[0051] (2) Crushing method

[0052] The number of rice crushing is not only related to the size of the particles, but also related to the uniformity of the particles. The influence of crushing times on the precision of the method was investigated by calculating the relative standard deviation (RSD) of 5 parallel samples, and the results ...

Embodiment 3

[0064] (1) Preparation of standard curve and method evaluation

[0065] Add standard substances of different gradients dissolved in ethanol to the rice sample in the headspace bottle. After using the instrument for detection, take the sample without adding the standard as the blank, and measure the peak area of ​​each aldehyde after the addition of the standard. After standardization, the peak area increase value of each component is y, and the scalaring amount is x, and a standard curve is drawn, and the standard curve is forced to pass through the origin. The results showed that the optimal standard addition volume was 5 μL, and the standard curves of each aldehyde had good linearity within their respective linear ranges (2-1000 μg / kg), with R2 greater than 0.99, which could meet the requirements of accurate quantitative analysis. The results are shown in Table 3. The samples in the headspace vial were added with and without 5 μL of ethanol, and the results showed that the a...

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Abstract

The invention discloses a method for detecting aldehydes in rice. According to the method, the method is realized by employing a headspace derived solid phase micro-extraction-gas chromatography-mass spectrometry method. The method comprises the following steps of: grinding a rice sample, adding the detected sample into a headspace bottle, introducing protective gas, inserting an extraction head into the headspace bottle filled with derivative liquid for deriving for 20 minutes, and inserting the extraction head into a headspace sample introduction bottle, wherein the extraction temperature is 40 DEG C, and the extraction time is 80 minutes; detecting in a gas chromatograph-mass spectrometer. The fineness and headspace derivatization conditions of the ground rice particles are optimized, so that newly generated aldehydes in the analysis process are avoided, and the accuracy of an experimental result is improved. According to the detection method, five steps of adsorbing derivative liquid of the extraction head, deriving and extracting the aldehydes, performing sample introduction, separating and measuring can be sequentially finished in a process, automation is realized, the operation is simple, the detection efficiency and accuracy are improved, and absolute quantification of nine aldehydes in rice is realized.

Description

technical field [0001] The invention relates to an analysis and detection method for aldehyde substances, in particular to a detection method for aldehyde substances in rice. Background technique [0002] With the continuous improvement of people's living standards, the quality of rice has been paid more and more attention. The aromatic flavor substances of rice have gradually become a characteristic favored by consumers, and volatile flavor substances have been identified as one of the important factors to evaluate the quality of rice at home and abroad. The volatile content of aldehydes is an important index to evaluate the taste and freshness of rice, and it has been a research hotspot at home and abroad for more than 20 years. The content of aldehydes in fresh rice changes greatly after being stored for a period of time, and valeraldehyde and hexanal are usually the main components of the unpleasant smell of old rice. [0003] At present, the following three methods ar...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 樊伟杨理章董建军尹花郝俊光陆健郑敏田玉红闫鹏陈华磊
Owner TSINGTAO BREWERY
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