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Internal Standard Determination Method of Benzene and Benzene Series in Glycerol Triacetate Using Headspace-Gas Mass Spectrometry

A technology for the determination of glyceryl acetate and its determination method, which is applied in the field of triethylamine using headspace-gas chromatography mass spectrometry, can solve the problems of cumbersome and time-consuming sample processing, and achieve simplified pre-processing steps, reduced cumbersome operations, and reduced errors and operations. cumbersome effect on

Active Publication Date: 2016-11-23
CHINA TOBACCO GUANGDONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method sample processing is cumbersome and time-consuming

Method used

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  • Internal Standard Determination Method of Benzene and Benzene Series in Glycerol Triacetate Using Headspace-Gas Mass Spectrometry
  • Internal Standard Determination Method of Benzene and Benzene Series in Glycerol Triacetate Using Headspace-Gas Mass Spectrometry
  • Internal Standard Determination Method of Benzene and Benzene Series in Glycerol Triacetate Using Headspace-Gas Mass Spectrometry

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: Establish the internal standard determination method of benzene and benzene series in glycerol triacetate of headspace-gas chromatography mass spectrometry

[0038] S1. Preparation of standard working solution: Accurately weigh 100 mg each of benzene, toluene, ethylbenzene, o-xylene, m-xylene, and p-xylene in a 50 mL volumetric flask, and dilute to volume with chromatographically pure glycerol triacetate to obtain 2 mg / mL primary mixed standard stock solution; pipette 50 μL and dilute to 10 mL to obtain a secondary mixed standard stock solution with a concentration of each component of 10 ug / mL. Accurately pipette 10, 20, 40, 100, 200, 500 μL of 10 ug / mL secondary mixed standard stock solution into six 10 mL volumetric flasks, add 5 μL of 2 mg / mL IS solution respectively, and use chromatographically pure triacetic acid Glyceride was fixed to 10 mL to obtain a series of standard working solutions with concentrations of 0.01, 0.02, 0.04, 0.1, 0.2, 0.5 μg / mL ...

Embodiment 2

[0052] Embodiment 2 Practical application example

[0053] Other operations and conditions are the same as in Example 1, and 5 triacetin samples are randomly selected as detection and analysis objects, and other operations are the same as in Example 1. The test results are shown in Table 3:

[0054] Table 3 Detection results of benzene and benzene series in samples

[0055]

[0056] Repeatability and recovery experiment results are shown in Table 4:

[0057] Table 4 Test results

[0058] compound

[0059] The invention determines the scientific headspace treatment conditions, and completes the treatment of the sample solution. After the sample is scientifically and reasonably processed by the headspace instrument of the invention, it is directly introduced into the gas chromatography mass spectrometry analysis, which effectively reduces the errors and operations caused by the pretreatment. Compared with the sample pretreatment method of the existing analysis an...

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Abstract

The invention discloses a method for internal standard determination of benzene and benzene series in glyceryl triacetate through headspace-gas mass spectrometry. According to the method disclosed by the invention, benzene and benzene series in glyceryl triacetate are determined through headspace-gas mass spectrometry; an internal standard method is adopted for quantification, and through such optimization measures as chromatographically pure glyceryl triacetate which simultaneously serves as a solvent and a matrix correcting agent and sample pretreatment, detection chromatographic conditions are determined in a targeted manner and a chromatographic peak separation effect among benzene, methyl benzene, ethyl benzene, o-xylene, m-xylene and m-xylene is better guaranteed, and the method has good linear dependence. Detected by the method disclosed by the invention, detection limit of benzene and benzene series is 0.01mu g / mL, relative standard deviation is 1.4-3.6% and recovery rate is 84.1-98.3%; and error and complex operation caused by sample pretreatment are effectively reduced, and treatment time is also greatly shortened.

Description

technical field [0001] The present invention relates to the technical field of detection, and more specifically, to a triethylamine using headspace-gas mass spectrometry [0002] Internal standard determination method of benzene and benzene series in glycerides. Background technique [0003] Glycerin triacetate is applied to the tow to prepare a filter rod, which is tipped and packed into a cigarette. The quality of glycerol triacetate not only affects the production and processing of filter rods and the physical indicators of filter rods, but also affects the quality and taste of cigarettes and the health of consumers. [0004] At present, the industrial production of glycerol triacetate usually adopts an acid-catalyzed synthesis method. In order to move the reaction to the direction of producing glycerol triacetate, benzene and benzene series are added. The determination of benzene and benzene series content in triacetin is of great significance to the quality of triacet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 穆小丽欧舟马丽娜
Owner CHINA TOBACCO GUANGDONG IND