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Gas chromatography-mass spectrometry method for determining content of 2-acetyl-1-pyrroline in fragrant rice leaves by external standard multipoint process

A technology of pyrroline and multi-point method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of many target interferences, time-consuming and labor-intensive, target loss, etc., to overcome cumbersome steps, good application prospects, and easy loss effect

Pending Publication Date: 2020-05-08
CHINA NAT RICE RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Rice odor analysis has been carried out at home and abroad for more than 20 years. Most of the literature on the collection of rice odor uses simultaneous distillation-extraction and adsorbent trapping methods. Disadvantages such as more interference
Recently, manual solid-phase microextraction technology has also been used. Although it directly extracts the target from the sample matrix, it integrates extraction, separation, concentration, and sample injection. It does not consume organic reagents and is easy to operate. However, due to the need to collect Then transfer to gas phase injection, there is a risk of target loss during the transfer, thereby reducing the concentration of sample characteristics
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 inlet, losses were likely to occur during the transfer process; and the amount of sample used was 8 g, The extraction time is 0.2 h, the sampling volume is large and it is easy to cause insufficient extraction, etc.

Method used

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  • Gas chromatography-mass spectrometry method for determining content of 2-acetyl-1-pyrroline in fragrant rice leaves by external standard multipoint process
  • Gas chromatography-mass spectrometry method for determining content of 2-acetyl-1-pyrroline in fragrant rice leaves by external standard multipoint process
  • Gas chromatography-mass spectrometry method for determining content of 2-acetyl-1-pyrroline in fragrant rice leaves by external standard multipoint process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0083] Step 1: The plants of rice variety 1 are taken from the top and first full leaves before heading, cut into pieces and immediately ground into powder with liquid nitrogen.

[0084] Step 2: Weigh 100 mg of the sample into a 20 ml screw top headspace vial and tighten it with a magnetic metal cap with a PTFE / blue silicone septum.

[0085] Step 3: Carry out the automatic solid-phase microextraction stage, and the extraction is divided into three stages:

[0086] The first stage: keep preheating at 70°C for 5 minutes.

[0087]The second stage: the type of extraction head adopts carbon molecular sieve / divinybenzene / polydimethylsiloxane (carboxen / divinybenzene / polydimethylsiloxane, CAR / DVB / PDMS; 50 / 30 µm, 1 cm long) at 70°C, with a rotation speed of 250 rpm / min. The depth of the extraction head into the vial is 18 mm. This extraction phase lasted 30 min.

[0088] The third stage: the extract was directly injected into the injection port of the GC-MS instrument, the inject...

Embodiment 2

[0097] Step 1: The flag leaves after heading are taken from the plants of rice variety 2 and ground with liquid nitrogen.

[0098] Step 2: Weigh 100 mg of the sample into a 20 ml screw top headspace vial and tighten it with a magnetic metal cap with a PTFE / blue silicone septum.

[0099] Step 3: Carry out the automatic solid-phase microextraction stage, and the extraction is divided into three stages:

[0100] The first stage: keep preheating at 80 ℃ for 10 min.

[0101] The second stage: the type of extraction head adopts carbon molecular sieve / divinybenzene / polydimethylsiloxane (carboxen / divinybenzene / polydimethylsiloxane, CAR / DVB / PDMS; 50 / 30 µm, 1 cm long) at 80 ℃, rotating speed 220 rpm / min, shake for 20 s, and stop for 5 s at intervals. The depth distance of the extraction head into the vial is 22 mm. This extraction phase lasted 40 min.

[0102] The third stage: the extract was directly injected into the injection port of the GC-MS instrument, the injection time was...

Embodiment 3

[0112] Step 1: The plants of rice variety 3 are taken from flag leaves after heading, and ground with liquid nitrogen.

[0113] Step 2: Weigh 100 mg of the sample into a 20 ml screw top headspace vial and tighten it with a magnetic metal cap with a PTFE / blue silicone septum.

[0114] Step 3: Carry out the automatic solid-phase microextraction stage, and the extraction is divided into three stages:

[0115] The first stage: keep preheating at 80 ℃ for 15 minutes.

[0116] The second stage: the type of extraction head adopts carbon molecular sieve / divinybenzene / polydimethylsiloxane (carboxen / divinybenzene / polydimethylsiloxane, CAR / DVB / PDMS; 50 / 30 µm, 1 cm long) at 80 ℃, rotating speed 250 rpm / min. The depth of the extraction head into the vial is 23 mm. This extraction phase lasted 50 min.

[0117] The third stage: the extract was directly injected into the injection port of the GC-MS instrument, the injection time was 1.5 min, and the injection temperature was 250°C.

...

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PUM

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Abstract

The invention relates to the field of food detection, and discloses a gas chromatography-mass spectrometry method for determining the content of 2-acetyl-1-pyrroline in fragrant rice leaves by an external standard multi-point process. The method comprises: S1: sampling; S2: leaf pretreatment and sample weighing; S3: solid-phase microextraction pretreatment; S4: gas chromatography-mass spectrometryanalysis; S5: establishment of a 2-acetyl-1-pyrroline external standard multi-point process; S6: establishment of a relative recovery factor RRF; and S7: formula calculation. The data repeatability standard deviation (referring to a same extraction head) of the obtained sample is smaller than 1.5%, the reproducibility standard deviation is smaller than 8.5%, the sample detection concentration is0.0035mg / kg, and the quantitative detection limit (S / N = 10) is 0.001mg / Kg. The method provided by the invention is simple, convenient, quick, accurate, low in cost and efficient, and has good application prospects in fragrant rice quality early identification, fragrant gene genetic research and breeding early generation screening.

Description

technical field [0001] The invention relates to the field of food testing, in particular to a gas-phase mass spectrometry method for measuring the content of 2-acetyl-1-pyrroline in fragrant rice leaves by an external standard multi-point method. Background technique [0002] Fragrant rice is deeply loved by consumers for its refreshing aroma, and the price of high-quality fragrant rice in the market is much higher than that of ordinary rice. There are many varieties of fragrant rice in China, and there are more than 200 kinds of aroma volatiles in fragrant rice, among which 2-acetyl-1-pyrroline (2AP) is the main aroma characteristic volatile (Lin et al., 1990; Ahmed et al., 1995; Tanchotikul and sieh, 1991; Maraval et al, 2008; Mathure et al, 2014), with a popcorn scent. [0003] Rice odor analysis has been carried out at home and abroad for more than 20 years. Most of the literature on the collection of rice odor uses simultaneous distillation-extraction and adsorbent tra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/025
Inventor 谢黎虹唐绍清胡培松魏祥进邵高能焦桂爱圣忠华
Owner CHINA NAT RICE RES INST
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