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A method for simultaneous detection of six synthetic sweeteners in tea

A technology for sweeteners and tea leaves, applied in the field of chemical analysis, can solve problems such as difficulty in application, complex tea matrix components, and inability to measure synthetic sweeteners at the same time, achieving simple operation, avoiding multiple extraction operations, and good purification effect. Effect

Active Publication Date: 2021-03-09
TEA RES INST CHINESE ACAD OF AGRI SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the composition of tea substrates is complex, which is quite different from these substrates, and it is difficult to apply the method directly to tea.
Other standard methods, such as "Determination of Benzoic Acid, Sorbic Acid and Sodium Saccharin in Food Safety National Standard Food" (GB 5009.28-2016), "Determination of Neotame in Food Safety National Standard Food" (GB5009.247-2016) and "Determination of Aspartame and Alitame in Food Safety National Standard Food" (GB5009.263-2016) is not dedicated to tea matrix and cannot simultaneously determine 6 synthetic sweeteners
In the existing published literature, the detection method of synthetic sweeteners is also mostly used in liquid tea beverages, not suitable for dry tea

Method used

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  • A method for simultaneous detection of six synthetic sweeteners in tea
  • A method for simultaneous detection of six synthetic sweeteners in tea
  • A method for simultaneous detection of six synthetic sweeteners in tea

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 1) Sample preparation

[0039] The tea samples were pulverized into powder by a pulverizer.

[0040] 2) Sample pretreatment

[0041] Accurately weigh 2.00 g of tea samples into a 50 mL stoppered centrifuge tube, add 20 mL of acetonitrile / water (1:1, v / v), shake on a shaker for 30 minutes, and centrifuge at 4700 rpm for 5 minutes. Pipette 1.00 mL of the supernatant to a 2 mL centrifuge tube containing 200 mg of graphitized carbon black or 50 mg of multi-walled carbon nanotubes or 100 mg of graphitized carbon black mixed with 25 mg of multi-walled carbon nanotubes, vortex for 1 minute, and centrifuge at 15,000 rpm for 5 Minutes, take 1 mL of the supernatant and pass it through a nylon filter (13 mm, 0.22 μm), and the resulting filtrate is used as a sample solution for analysis by liquid chromatography-tandem mass spectrometry.

[0042] 3) Standard solution preparation

[0043] A blank sample solution was obtained by using a blank tea sample that does not contain 6 targ...

Embodiment 2

[0054] Addition and recovery tests were carried out on the detection methods using 3 different dispersive solid phase extraction adsorbents. Green tea and black tea were used as substrates respectively, and the addition levels of 6 synthetic sweeteners were 0.1mg / kg, 1mg / kg and 10mg / kg. .

[0055] The results of the addition recovery test are shown in Table 3. When graphitized carbon black was used as dispersive SPE adsorbent, the average recoveries of the six synthetic sweeteners in green tea were 92.9%-106.9%, and the relative standard deviations were all less than 3.8%; The average recoveries were 84.4%-99.5%, and the relative standard deviations were all less than 4.4%. When multi-walled carbon nanotubes were used as dispersive SPE adsorbents, the average recoveries of the six synthetic sweeteners in green tea were 89.5%-99.9%, and the relative standard deviations were all less than 4.6%; the six synthetic sweeteners in black tea The average recoveries were 86.2%-102.2%,...

Embodiment 3

[0060] To verify the linear relationship of 6 synthetic sweeteners using 3 different dispersive SPE sorbents, the prepared concentrations were 0.0005mg / L, 0.001mg / L, 0.005mg / L, 0.01mg / L, 0.05 mg / L, 0.1mg / L, 0.5mg / L, 1mg / L green tea and black tea matrix matching standard solution, with 1 / c s Fit a linear standard curve to the weights. The concentration in the sample at which the converted signal-to-noise ratio was 10 was the quantitation limit of the method.

[0061] The linear relationship and limit of quantification of the standard curve are shown in Table 4. Within the corresponding linear range, the linear correlation coefficients of the six sweeteners in green tea and black tea were all greater than or equal to 0.9990, and the three methods had good linear relationships. When graphitized carbon black is used as the dispersive SPE adsorbent, the quantitative limits of cyclamate, saccharin sodium, acesulfame potassium, aspartame, alitame and neotame in green tea and black ...

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Abstract

The invention discloses a method for simultaneously detecting six synthetic sweeteners in tea leaves. The method is as follows: tea samples are extracted with an acetonitrile-water mixed solution with a volume ratio of 1:1, and then an adsorbent is added to disperse the sample extracts Solid-phase extraction purification, the adsorbent is graphitized carbon black or multi-walled carbon nanotubes or a mixture of the two, and then analyzed by liquid chromatography-tandem mass spectrometer, in negative ion mode, for multiple reaction monitoring determination, according to the standard Curve and external standard method quantify, detect and calculate and obtain the content of 6 kinds of synthetic sweeteners in the tealeaves; Said 6 kinds of synthetic sweeteners are sodium cyclamate, sodium saccharin, acesulfame potassium, aspartame, alitame or neodymium sweet. The method of the present invention only needs to extract tea samples once, is easy to operate, is suitable for processing large batches of samples in a single experiment, has good purification effect, reduces the pollution to the instrument, and can complete the simultaneous detection of 6 synthetic sweeteners in one sample analysis , enabling high-throughput detection.

Description

technical field [0001] The invention belongs to the technical field of chemical analysis methods, and in particular relates to a method for detecting six synthetic sweeteners in tea. Background technique [0002] The sensory quality of tea includes appearance, soup color, taste, aroma and leaf bottom, among which taste and aroma play an important role. According to the "GB 2760-2014 Food Safety National Standard for the Use of Food Additives" and tea-related product standards, no food additives can be used in tea; although food additives can be used in flavored teas, the only additives currently allowed are steviol glycosides. However, due to reasons such as the climate of the producing area, the season of picking, the tenderness of fresh leaves, and the processing technology, some tea leaves and the seasoning teas made from them have poor sensory quality, insufficient aroma, and heavy bitter and astringent taste. Tea producers have an incentive to improve the taste and aro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 王晨诸力刘新鲁成银
Owner TEA RES INST CHINESE ACAD OF AGRI SCI