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Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry

A technology of time-of-flight mass spectrometry and ultra-high pressure liquid phase, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems that cannot be dealt with and the detection sensitivity needs to be improved, and achieve high sensitivity, simple and fast analysis method, and good selectivity Effect

Active Publication Date: 2012-06-27
上海国矗生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is basically determined for a single sweetener or two sweeteners, and the detection sensitivity needs to be improved. It cannot cope with the phenomenon that some companies add a variety of sweeteners at the same time in order to evade supervision.

Method used

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  • Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry
  • Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry
  • Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0062] The following examples will specifically illustrate the operation method of the present invention, but should not be regarded as a limitation of the present invention. Example 1 Detection of a certain brand liquor sweetener in the market

[0063] 1 material

[0064] 1.1 Instruments

[0065] Ultra-high pressure liquid chromatography: WATERS ACQUITY UPLC, detector: WATERS ACQUITYPDA, chromatographic column: BEH C-18 2.1mm×50mm 1.7um, time-of-flight mass spectrometer: WATERSSYNAPT MS, Masslynx 4.1 mass spectrometry management software.

[0066] 1.2 Reagents and samples

[0067] Methanol: chromatographically pure (Sinopharm Group); 20mmol / L ammonium acetate solution: Dissolve 1.54g of ammonium acetate (Sinopharm Group) in ultrapure water to 1000ml, and then filter through a 0.2μm filter membrane; Standard samples of six sweeteners: saccharin The purity of sodium, sodium cyclamate, and acesulfame potassium is 99.9% (Sigma Company, USA); Aspartame purity is 99.0% (Sigma Co...

example 2

[0104] Example 2 Detection of a certain brand liquor sweetener in the market

[0105] A commercially available liquor sample of another brand was detected by substantially the same method as in Example 1 above. In Example 2, the pretreatment method, chromatographic mass spectrometry conditions, detection instrument, and standard curve were all referred to in Example 1.

[0106] Result analysis

[0107] Chromatograms from six sweetener standards ( Figure 7 ) as can be seen, the retention time of sodium saccharin, one of the six sweeteners, was 2.43 min, and the sample ( Figure 16 ), there is a chromatographic peak at 2.41min and the retention time of the chromatographic peak of sodium saccharin is similar, so the sample chromatogram can be preliminarily determined ( Figure 16 ) in the chromatographic peak at 2.41min is sodium saccharin. Then according to the sample, the characteristic molecular ion peak at m / z=182 ( Figure 9 ), which is the same as the characteristic mo...

example 3

[0110] Example 3 Detection of sweeteners of a certain brand of liquor on the market

[0111] Detected another commercially available liquor sample in the same manner as in Example 1 above. In Example 3, pretreatment methods, chromatographic mass spectrometry conditions, detection instruments, and standard curves were all with reference to Example 1.

[0112] Result analysis

[0113] The chromatogram ( Figure 7 ) It can be seen that the retention times of acesulfame-K, sodium saccharin, and cyclamate are respectively 1.75min, 2.43min, and 2.91min among the six sweeteners, and the samples ( Figure 18 ) in 1.73min, 2.43min, 2.91min chromatographic peaks can be preliminarily judged as three kinds of sweeteners of acesulfame potassium, saccharin sodium, sodium cyclamate, and then according to the sample at the corresponding retention time respectively m / z=162 ( Figure 19 ), m / z=178, m / z=182 characteristic molecular ion peaks are consistent with the characteristic molecular ion...

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Abstract

The invention relates to a method for detecting six trace sweetening agents in white spirit by an ultra-high pressure liquid chromatography-time-of-flight mass spectrometry (UPLC-TOF-MS) technology. Particularly, the invention adopts the UPLC-TOF-MS technology and specially aims at the phenomenon of trace addition of a plurality of sweetening agents in the current white spirit industry. The invention can detect six sweetening agents of acesulfame-K, soluble saccharin, sodium cyclamate, sucralose, aspartame and neotame simultaneously, is rapid, simple and convenient, has accurate qualificationand quantification and high sensitivity and effectively solves the problem. The method has the detection limit of the acesulfame-K of 0.05mg / L, the detection limits of the soluble saccharin, the sodium cyclamate and the neotame of 0.01 mg / L and the detection limits of the sucralose and the aspartame of 0.1 mg / L, only needs 10 min of one-step sampling analysis and has favorable linear relation andrepeatability. Compared with detection data of an authority depart, the data detected by the method is also accurate and reliable.

Description

technical field [0001] The invention relates to a method for simultaneously detecting six trace sweeteners in liquor by using ultra-high pressure liquid chromatography and time-of-flight mass spectrometry. The invention belongs to the technical field of chemical analysis and instrumental analysis in the fermented food industry. Background technique [0002] Sweetener is an important class of food additives, it endows food with sweetness, improves the quality of food, has the advantages of low calorie, suitable for people with diabetes and so on. Sweeteners can be divided into natural sweeteners and artificial sweeteners according to their sources. The synthetic sweeteners widely used in the modern food industry mainly include acesulfame potassium (Acesulfame-K, Acesulfame-K), o-benzoylsulfonamide sodium (saccharin sodium, Saccharin sodium), cyclamate sodium (Sodium cyclamate), sucralose (Sucralose), aspartame (Aspartame, Aspartame) and N-[N-(3,3-dimethyl Butyl)-L-α-aspart...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/36
Inventor 王洪新吴世嘉陶冠军
Owner 上海国矗生物科技有限公司
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