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Simplified gas chromatography-mass spectrometry method for quantifying the content of 2-acetyl-1-pyrroline, a characteristic aroma substance in fragrant rice

A characteristic substance, pyrroline technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of high dosage, easy decomposition, difficulty, etc., and achieve the effect of good data repeatability, difficult decomposition and high accuracy

Active Publication Date: 2018-09-21
CHINA NAT RICE RES INST
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Problems solved by technology

For example, domestic Ying Xinghua et al. (Journal of Analytical Testing, 2011, 27, 69-71) reported that after manual solid phase microextraction was transferred to the gas phase injection port, losses were likely to occur during the transfer process; and the amount of sample used was 8g, and the extraction The time is 0.2h, it is easy to cause insufficient extraction, etc.
For example, 1991 Tanchotikul and Hsien (J.Agric.Food Chem, 1991,39,944-947) abroad reported quantitative 2-AP with a gas phase-mass spectrometer, but the distillation and reagent extraction methods used for pretreatment, the internal standard TMP was directly added Samples are pre-treated together, which not only easily causes losses such as target decomposition, but also requires a sample dosage of 1g
In 2001, Mahatheeeranont (J.Agric.Food Chem, 2001,49,773-779) etc. reported the use of vacuum indirect distillation and reagent extraction. The previous treatment could reduce the loss of the target substance caused by the boiling of the reagent, but it did not completely prevent other non-products of the target substance. Decomposition and other losses caused by high temperature; and the amount of sample and internal standard TMP reached 0.5g and 0.008mg respectively, the amount of addition is high, and the conversion factor of TMP is not considered in the quantification (that is, direct injection and pre-treatment injection The ratio of peak efficiency)
In 2001, Grimm et al. (J.Agric.Food Chem, 2001,49,245-249) reported using automatic solid-phase microextraction, but the amount of sample was still as high as 0.75g, and the recovery rate of TMP in this quantitative method was less than 0.3%
The former uses 2,6-Dimethylpyridine as an internal standard, and the latter uses 2AP-d 2 As an internal standard; 2-AP is used as a quantitative standard curve; because 2-AP is unstable and easy to decompose, and this pure product is not easy to obtain, it is difficult in actual general laboratory operations
Sriseadka et al. 2006 In order to avoid the decomposition of 2-AP, the extraction temperature of the sample was only 27°C, and this temperature is not efficient for the extraction of 2-AP in rice flour

Method used

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  • Simplified gas chromatography-mass spectrometry method for quantifying the content of 2-acetyl-1-pyrroline, a characteristic aroma substance in fragrant rice
  • Simplified gas chromatography-mass spectrometry method for quantifying the content of 2-acetyl-1-pyrroline, a characteristic aroma substance in fragrant rice
  • Simplified gas chromatography-mass spectrometry method for quantifying the content of 2-acetyl-1-pyrroline, a characteristic aroma substance in fragrant rice

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Embodiment 1

[0038] A gas-phase-mass spectrometry method for quantitatively simplifying the content of 2--acetyl-1-pyrroline (2-AP), a characteristic aroma substance of aromatic rice, comprising the following steps:

[0039] Step 1: the pretreatment of rice flour, brown rice is ground into the rice flour of crossing 0.42mm fineness sieve;

[0040] Step 2: The sample weight is 50 mg, add 2,4,6 collidine (TMP) as the internal standard, the addition amount is 20 ng, put it into a 20 ml screw headspace sample bottle, and use a PTFE / blue silica gel septum The pad's magnetic metal cover screws on.

[0041] Step 3: Carry out automatic solid-phase microextraction stage, extraction is divided into three stages:

[0042] The first stage: keep preheating at 80°C for 10 minutes;

[0043] The second stage: the extraction head model is fiber (carboxen / divinybenzene / polydimethylsiloxane, CAR / DVB / PDMS; 50 / 30μm, 1cm long) at 80°C, rotating speed 250rpm / min, shaking for 20S, and stopping for 5S at interva...

Embodiment 2

[0058] A gas-phase-mass spectrometry method for quantitatively simplifying the content of 2--acetyl-1-pyrroline (2-AP), a characteristic aroma substance of aromatic rice, comprising the following steps:

[0059] Step 1: pretreatment of rice flour, brown rice is ground into rice flour with a fineness sieve of 0.59mm;

[0060] Step 2: The sample weight is 100 mg, add 2,4,6 collidine (TMP) as the internal standard, the addition amount is 5 ng, put it into a 20 ml screw headspace sample bottle, and use a PTFE / blue silica gel septum The pad's magnetic metal cover screws on.

[0061] Step 3: Carry out automatic solid-phase microextraction stage, extraction is divided into three stages:

[0062] The first stage: keep preheating at 80°C for 10 minutes;

[0063] The second stage: the extraction head model is fiber (carboxen / divinybenzene / polydimethylsiloxane, CAR / DVB / PDMS; 50 / 30μm, 1cm long) at 80°C, rotating speed 250rpm / min, shaking for 20S, and stopping for 5S at intervals. The d...

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Abstract

In order to use an automatic solid-phase microextraction injector, simplify quantification of the content of fragrance characteristic 2-acetyl-1-pyrroline of fragrant rice, overcome tedious steps and easily losing problems that transfer sample introduction is performed after manual solid phase microextraction is performed, and solve the low synthesis purity and unstable problem of a 2-AP substance, the invention provides a gas chromatography-mass spectrometry method for simplifying quantification of the content of the fragrance characteristic 2-acetyl-1-pyrroline of the fragrant rice. A standard curve is directly made by TMP, and is used to carry out quantitative analysis on the 2-acetyl-1-pyrroline content. The repeatability is good, and the detecting limit is low. The gas chromatography-mass spectrometry method for simplifying quantification of the content of the fragrance characteristic 2-acetyl-1-pyrroline of the fragrant rice has good application prospects on rice quality improvement, fragrance genetic research and food fragrance technology.

Description

technical field [0001] The invention relates to a method for detecting aroma substances, in particular to a gas phase mass spectrometry method for simplifying and quantifying the content of 2-acetyl-1-pyrroline, a characteristic aroma substance of fragrant rice. Background technique [0002] Fragrant rice is loved by domestic and foreign consumers for its delicate fragrance and delicious taste. The price of high-quality fragrant rice in the market is generally 2 to 3 times that of ordinary rice. Fragrant rice is rich in resources and has a long history of cultivation. It is found in almost all rice-producing countries in the world. India, Thailand, Pakistan, Vietnam, Japan and the United States all have their own high-quality fragrant rice varieties; such as Basmati fragrant rice in India. , Thailand's Khao Dawk Mail105, Australia's Goolarah, America's Della, Iran's Sadri, Japan's Congratulations, and China's Wannian fragrant rice are all famous varieties of fragrant rice. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 谢黎虹胡培松唐绍清魏祥进邵高能焦桂爱圣忠华
Owner CHINA NAT RICE RES INST
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