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Method for detecting ester components in orange juice by online solid-phase micro-extraction and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry

A technology of two-dimensional gas chromatography and quadrupole mass spectrometry, which is applied in the field of detection of ester components in orange juice, can solve the problems of inability to separate components and limited separation ability of one-dimensional gas chromatography, and achieve high-efficiency separation

Inactive Publication Date: 2014-08-20
ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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Problems solved by technology

[0005] The existing method for detecting esters in fruit juice adopts traditional one-dimensional gas chromatography-mass spectrometry. The separation ability of one-dimensional gas chromatography is limited, and all components cannot be completely separated. A single analysis may only analyze dozens of compounds. However, comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry can detect hundreds of compounds, and its peak capacity is hundreds to thousands of times that of one-dimensional liquid chromatography-mass spectrometry.

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  • Method for detecting ester components in orange juice by online solid-phase micro-extraction and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry
  • Method for detecting ester components in orange juice by online solid-phase micro-extraction and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry
  • Method for detecting ester components in orange juice by online solid-phase micro-extraction and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry

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Embodiment Construction

[0045] Below in conjunction with accompanying drawing and specific embodiment the present invention is described in further detail:

[0046] 1. Instruments and reagents

[0047] Instrument: Shimadzu Q2010 Ultra GC / GC / MS with AOC-5000 Plus autosampler

[0048]Acetonitrile, sodium chloride, analytically pure. C8-C20 normal alkanes standard (Sigma-Aldrich, 1mL)

[0049] 2. Sample processing

[0050] Weigh 5 g of freshly squeezed orange juice into a 10 mL headspace vial, add 2 g of NaCl, and seal it with a cap. Fully automatic solid-phase microextraction and fully automatic sample injection methods are used for sample enrichment and analysis. The online solid-phase microextraction conditions are: the extraction head is an 85 μm Polyacrylate automatic extraction head; the sample incubation temperature is 45 o C; incubate for 10 min to equilibrate; insert the extraction head into the vial to a depth of 12 mm; extract for 20 min.

[0051] 3. Instrument conditions

[0052] The ...

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Abstract

The invention discloses a method for detecting ester components in orange juice by online solid-phase micro-extraction (online-SPME) and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry (Comprehensive 2D GC / qMS). The method comprises the following steps: enriching ester components in an orange juice sample by online-SPME and detecting by comprehensive 2D GC / qMS; carrying out qualitative analysis on a detected compound in a manner of combining retention indexes and an NIST spectral library; and accurately quantifying chromatography overlapping peaks of components, which can not be separated by comprehensive 2D GC / qMS, by section convolution. According to comprehensive 2D GC / qMS, two chromatographic columns with different polarities are used to carry out orthogonal separation on the ester components and then the separated components enter qMS under the effect of a modulator-demodulator to be detected; the retention time indexes and the NIST spectral library are combined to carry out qualitative analysis; a section convolution technology is used for quantifying the chromatography overlapping peaks accurately. The method has the characteristics of high throughput, high sensitivity and high accuracy; the problems that the analysis and the separation of ester components of orange juice are difficult and the qualitative analysis is difficult are solved.

Description

technical field [0001] The invention belongs to the technical field of food safety, and relates to a method for detecting ester components in orange juice by applying online solid-phase microextraction and comprehensive two-dimensional gas chromatography-quadrupole mass spectrometry. Background technique [0002] Orange juice is rich in nutrition and has a pleasant aroma. It is a popular and widely consumed beverage in the world. Among them, orange juice, as the main orange juice drink, ranks first in the world in consumption. In recent years, orange juice and its beverage industry have achieved great development with the improvement of people's recognition. However, due to the lack of corresponding quality control system, the phenomenon of quality adulteration, deception, and harmful substances exceeding the standard still occurs from time to time. [0003] The current national standard for the monitoring of orange juice safety mainly includes basic physical and chemical i...

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Application Information

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IPC IPC(8): G01N30/88
Inventor 郑文杰李淑静何佳陈其勇宓捷波王云凤张晓许泓
Owner ANIMAL & PLANT & FOOD INSPECTION CENT OF TIANJIN ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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