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Method for simultaneously detecting three monoglyceride emulsifiers in dairy product based on gas chromatography-mass spectrometry

A technology of gas chromatography and dairy products, applied in the field of simultaneous detection of three monoglyceride emulsifiers in dairy products, which can solve the problems of low detection sensitivity and complicated processing process

Pending Publication Date: 2020-12-01
NANCHANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These analytical methods have defects such as complicated sample pretreatment process and low detection sensitivity.

Method used

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  • Method for simultaneously detecting three monoglyceride emulsifiers in dairy product based on gas chromatography-mass spectrometry
  • Method for simultaneously detecting three monoglyceride emulsifiers in dairy product based on gas chromatography-mass spectrometry

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Effect test

Embodiment 1

[0020] Gas chromatography-mass spectrometry (USA, Agilent Corporation), including 7080B chromatographic system, 5977MSD and NIST spectral retrieval library. Chromatographic conditions: chromatographic column: HP-5MS capillary column; heating program: initial temperature is 60 °C, rising to 270 °C at 30 °C / min, rising to 285 °C at 3 °C / min; carrier gas: high-purity helium; flow rate: 1.0 mL / min; injection volume: 1.0 μL; split ratio: 10:1; inlet temperature: 250 °C. Mass spectrometry conditions: electron bombardment (EI) ion source; electron energy: 70 eV; ion source temperature: 230 ℃; quadrupole temperature: 150 ℃; solvent delay: 6.5 min; acquisition method: selected ion scanning. The mass spectrometric detection parameters of the three target compounds are shown in Table 1.

Embodiment 2

[0022] CH in Dairy 2 Cl 2 The extract is used as a solvent, and a series of mass concentrations of glyceryl monopalmitate, glyceryl monooleate and glyceryl monostearate are prepared as a standard working solution of mixed matrix, and the silylating reagent N,O-bis(trimethylsilyl) After derivatization with trifluoroacetamide (containing trimethylchlorosilane) (BSTFA+1%TMCS), the analysis was carried out under the above chromatographic and mass spectrometric conditions, and the peak area (y) was used to perform linear regression on the analyte concentration (x). The equation, detection limit and quantification limit are shown in Table 2.

Embodiment 3

[0024] Sample pretreatment: Accurately weigh about 0.5 g of milk sample, add 5.0 mL of water and mix well; add 10.0 mL of CH 2 Cl 2 For extraction, shake for 10 min. Centrifuge at 13000 r / min for 10 min, and collect the lower organic phase. Then add 10.0mLCH 2 Cl 2 The above extraction steps were repeated, and the organic phases were combined. Take 1.0 mL of extract liquid and dry it with nitrogen gas, add 50 μL of pyridine to dissolve; then add 100 μL of silylating reagent N,O-bis(trimethylsilyl)trifluoroacetamide (containing trimethylchlorosilane) (BSTFA+1% TMCS), react at 70 °C for 40 min, and dilute to 1.0 mL with n-heptane to obtain the upper machine solution.

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Abstract

The invention discloses a method for simultaneously detecting three monoglyceride emulsifiers in a dairy product based on gas chromatography-mass spectrometry. The method comprises the steps of gas chromatography-mass spectrometry conditions; detecting the glyceryl monopalmitate, the glyceryl monooleate and the glyceryl monostearate; pretreating a sample; and detecting the sample. According to themethod, a simple liquid-liquid extraction method is adopted, a GC-MS analysis technology is combined, a novel method for analyzing the three monoglyceride emulsifiers in the dairy product is provided, the instrument detection limit ranges from 0.26 mg / L to 1.20 mg / L, and a novel technical means is provided for dairy product quality supervision.

Description

technical field [0001] The invention belongs to the technical field of analysis, and in particular relates to a method for simultaneously detecting three monoglyceride emulsifiers in dairy products based on gas chromatography-mass spectrometry. Background technique [0002] Food emulsifiers are surfactants that make oil and water "miscible". Widely used in the processing of dairy products, bread, pastries, biscuits, margarine, ice cream, beverages, chocolate and other foods. [0003] Dairy products are one of the foods with high nutritional content in the human dietary structure, and a certain amount of emulsifiers are often added during their processing to stabilize their quality. At present, domestic and foreign researches on emulsifiers in dairy products mainly focus on the emulsifying properties of emulsifiers and the effect of the ratio of compound emulsifiers on the quality of dairy products. There are relatively few research reports on the detection of emulsifier co...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06G01N2030/047
Inventor 万益群罗芸鄢爱平刘翻郭岚
Owner NANCHANG UNIV
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