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Method for detecting trichloropropanol in corn oil by utilizing gas chromatograph-mass spectrometer

A gas spectrometry instrument and trichloropropanol technology, which is applied in the field of vegetable oil detection, can solve the problems of many consumables, complicated and fuzzy experimental process, and achieve scientific and reasonable detection methods, convenient quality control, and improved sensitivity.

Inactive Publication Date: 2018-11-02
SHANDONG SANXING CORN IND SCI CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

To detect trichloropropanol in corn oil, use the second method of this standard, but this method does not clarify whether corn oil can be detected, that is to say, there will be certain errors in the detection by the second method, which are all fuzzy boundaries
Moreover, the method has many consumables, and the experimental process is more complicated. It is not suitable for the detection of corn oil in enterprises. Facing the problems in the prior art, it is imperative to develop a method for detecting trichloropropanol in corn oil.

Method used

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  • Method for detecting trichloropropanol in corn oil by utilizing gas chromatograph-mass spectrometer
  • Method for detecting trichloropropanol in corn oil by utilizing gas chromatograph-mass spectrometer
  • Method for detecting trichloropropanol in corn oil by utilizing gas chromatograph-mass spectrometer

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Embodiment 1

[0035] Utilize the method for detecting trichloropropanol in corn oil by mass spectrometry, comprising the following steps:

[0036] 1) Determination of instrument testing conditions

[0037] Determine the chromatographic conditions as follows: Gas phase-mass spectrometry conditions Chromatographic column: HP-5MS column, 30m×0.25mm×0.25um; Injection port temperature: 250°C; To 165°C, hold for 10min, then raise to 300°C at a rate of 20°C / min, and hold for 8min, carrier gas: helium; splitless injection volume: 1.0uL, flow rate: 1ml / min.

[0038] Mass spectrometry conditions: ion source: electron bombardment mode (EI); transfer line temperature: 300 ° C; ion source temperature 230 ° C; MS quadrupole temperature 150 ° C; solvent delay 7min; selected ion monitoring mode (SIM) parameters: 3-MCPD Phenylboronic acid derivatives (m / z) 147 (quantitative ions), 146, 196, 198 (qualitative ions); 3-MCPD-d5 phenylboronic acid derivatives (m / z) 150 (quantitative ions), 149, 201, 203 (quali...

Embodiment 2

[0065] Utilize the method for detecting trichloropropanol in corn oil by mass spectrometry, comprising the following steps:

[0066] 1) Determination of instrument testing conditions

[0067] Determine the chromatographic conditions as follows: Gas phase-mass spectrometry conditions Chromatographic column: HP-5MS column, 30m×0.25mm×0.25um; Injection port temperature: 250°C; To 165°C, hold for 10min, then raise to 300°C at a rate of 20°C / min, and hold for 8min, carrier gas: helium; splitless injection volume: 1.0uL, flow rate: 1ml / min.

[0068] Mass spectrometry conditions: ion source: electron bombardment mode (EI); transfer line temperature: 300 ° C; ion source temperature 230 ° C; MS quadrupole temperature 150 ° C; solvent delay 7min; selected ion monitoring mode (SIM) parameters: 3-MCPD Phenylboronic acid derivatives (m / z) 147 (quantitative ions), 146, 196, 198 (qualitative ions); 3-MCPD-d5 phenylboronic acid derivatives (m / z) 150 (quantitative ions), 149, 201, 203 (quali...

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Abstract

The invention belongs to the technical field of oil detection and in particular relates to a method for detecting trichloropropanol in corn oil by utilizing a gas chromatograph-mass spectrometer. Thedetection method comprises the following steps: (1) determining instrument detection conditions; (2) preparing reagents and materials; (3) performing sample pretreatment; (4) establishing a marked line; and (5) calculating the trichloropropanol content. According to the method for detecting trichloropropanol in corn oil by utilizing the gas chromatograph-mass spectrometer disclosed by the invention, the detection sensitivity, accuracy and stability can be obviously improved, and the detection method is simple, rapid, stable and reliable. Meanwhile, the complicated process of existing nationalstandards at home at present is overcome, and the problem that an international technique for detecting the trichloropropanol in corn oil does not exist at present is solved. The method disclosed by the invention can be widely applied to determination of trichloropropanol in vegetable oil, is capable of realizing batch detection, and brings convenience to the quality control of trichloropropanol content in each vegetable oil production unit.

Description

technical field [0001] The invention belongs to the technical field of vegetable oil detection, and in particular relates to a method for detecting trichloropropanol in corn oil by using a gas spectrometer. Background technique [0002] Trichloropropanol is glycerol formed by the hydrolysis of fat under strong acid. Glycerol reacts under strong acid or high temperature conditions. HCL replaces the alcoholic hydroxyl group to generate chloropropanol, mainly 3-chloro-1,2-propanediol. Trichloropropanol has acute and chronic toxicity, mutagenicity and carcinogenicity. Its toxicity can cause tumors in some experimental animals, causing kidney and reproductive system damage. Therefore, the determination of trichloropropanol plays a very important role in practical work. The current determination of the content of trichloropropanol in food is mainly based on the method stipulated in the national standard GB / T5009.191--2006. To detect trichloropropanol in corn oil, use the second ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/88
CPCG01N30/06G01N30/88
Inventor 王月华刘玉兰王秀华毕小兰王萍程芳园成良玉
Owner SHANDONG SANXING CORN IND SCI CO LTD
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