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Method for measuring residual quantity of chloropicrin in fermented grain and white spirit

A technology of chloropicrin and fermented grains, applied in the field of chemical analysis, can solve the problems of long extraction time, cumbersome operation, inaccurate results, etc., achieve good linear relationship, avoid decomposition, and reduce the effect of sample interference

Active Publication Date: 2015-01-28
WULIANGYE
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the spectrophotometric method (GB / T 5009.36) is used for the determination of chloropicrin residues in grains. This method is cumbersome to operate and takes a long time to extract.
The colorimetric method is used in the determination process, so the interference is large, which can easily cause false positive or false negative, and the result is inaccurate
Using gas chromatography, the detector is ECD, and the extraction methods often use flow rate reflux and petroleum ether extraction, but they are all relatively cumbersome. Although the detection sensitivity of the ECD detector is very high, its qualitative only depends on the retention time of the peak. may cause false positive

Method used

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  • Method for measuring residual quantity of chloropicrin in fermented grain and white spirit
  • Method for measuring residual quantity of chloropicrin in fermented grain and white spirit
  • Method for measuring residual quantity of chloropicrin in fermented grain and white spirit

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Experimental program
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Effect test

Embodiment 1

[0026] a. Draw a standard curve: use 100ug / mL chloropicrin standard solution, use absolute ethanol as solvent, prepare 20ug / L, 50ug / L, 100ug / L, 500ug / L, 1000ug / L, 2000ug / L respectively Standard solution, after these solutions were injected into the GC-MS coupler for detection, the concentration-peak area standard curve was calculated according to the peak area of ​​each solution concentration and its corresponding M / Z 119, which was y=0.6741x+9.927, R 2 = 0.99924;

[0027] The gas chromatographic conditions of the GC-MS coupled instrument are: inlet temperature: 160°C, injection volume: 1μL, constant flow: 1.0mL / min, split mode: split ratio 8:1, transfer line temperature: 220°C 6min, then increase the temperature at 20℃ / min to 280℃ and keep for 10min; the mass spectrometry conditions are: ion source temperature 230℃, quadrupole temperature: 150℃, data acquisition mode: selected ions M / Z 117, M / Z 119, M / Z 121, in which M / Z 119 is used as the quantitative ion, the column tempe...

Embodiment 2

[0035] A, standard curve drawing is identical with embodiment 1; The condition of the gas chromatography of GC-MS coupler is identical with embodiment 1;

[0036] b. Weigh 6 samples of fermented grains fermented grains fermented for 10d, 30d, and 60d, each 5.00g into a 20mL test tube with a stopper, then accurately measure 5mL of absolute ethanol, shake well and put it into an ultrasonic extractor for ultrasonic extraction for 20min; use After filtration with 0.25um filter membrane, the filtrate is ready for use;

[0037] c, the standby filtrate of step b is injected into the GC-MS coupling instrument respectively to obtain the spectrogram of each fermented grains;

[0038] d. Analysis of chromatographic mass spectrogram: when the retention time was 4.998min, no fragment ion of m / z119 was detected, so the chloropicrin in each untested wine grain was not detected.

[0039] Calculated with a signal-to-noise ratio of 3 times, the detection limit of the instrument can reach 5ug / L...

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Abstract

The invention belongs to the technical field of chemical analysis and particularly relates to a method for measuring residual quantity of chloropicrin in fermented grains and white spirit, and aims to solve the technical problem about providing the method for measuring residual quantity of chloropicrin in the fermented grains and the white spirit. The method comprises the following steps: drawing a standard curve, introducing samples for detection, and analyzing a spectrogram to obtain a result. According to the method, the lower detection limit is 5 microgram / L, and one more accurate and effective method is provided for content determination of the chloropicrin in the fermented grains and the white spirit, so that a high foundation is laid for food safety of the white spirit.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis, in particular to a method for measuring residual chloropicrin in fermented grains and liquor. Background technique [0002] Chloropicrin is a warning fumigant that can kill insects, bacteria, and rodents. It can also be used for fumigation of food pests, wood preservation, building floors, ships, soil, and plant seeds. Colorless or yellowish oily liquid, lachrymatory, volatile, strong diffusivity, volatility increases with temperature rise. The chloropicrin vapor it produces is 5 times heavier than air. When the temperature is high, the medicinal effect is significant, and generally fumigation at 20°C is more appropriate. [0003] At present, the spectrophotometric method (GB / T 5009.36) is used for the determination of chloropicrin residues in grains. This method is cumbersome to operate and takes a long time to extract. The colorimetric method is used in the determination process, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 谢正敏彭智辅练顺才李杨华叶华夏赵东乔宗伟安明哲廖勤俭王小琴
Owner WULIANGYE
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