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Method for simultaneously determining sweetening agents and preservatives in tobacco essence

A technology for tobacco essence and sweetener, which is applied in the field of detection of chemical components of tobacco accessories, can solve the problems of difficult accurate determination of multiple components, difficult to achieve accurate determination of components, low component content, etc., and achieve high measurement efficiency and low sampling volume. Effect of less, lower limit of quantitation

Active Publication Date: 2016-05-25
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In actual work, liquid chromatography is often used for the joint determination of various sweeteners and preservatives in tobacco flavors, but liquid phase is rarely used for the determination of cyclamate (sodium cyclamate), mainly because cyclamate It is not absorbed in the range of ultraviolet and visible light. Pre-column derivatization must be carried out before HPLC measurement. The operation is cumbersome, and it is not easy to achieve accurate determination of multiple components.
[0006] Both sweeteners and preservatives are detected by liquid chromatography using ultraviolet detectors, and the quantification limits of each component are greater than 0.3 μg / mL. However, in actual samples, multiple components are added at the same time, and the content of some components may be low. Near or below the limit of quantitation, in which case it will be difficult to achieve accurate determination of all components
For example, the AS11HC analytical column is used for the determination of cyclamate in the industry standard, and the baseline of cyclamate and other ions can be separated by adjusting the column temperature and eluent concentration, but the linear range of the standard curve is only suitable for the determination of samples with a concentration greater than 10 μg / mL, and AS11HC It is still difficult for the analytical column to elute the two strong retained ions of acesulfame potassium and sodium saccharin

Method used

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  • Method for simultaneously determining sweetening agents and preservatives in tobacco essence
  • Method for simultaneously determining sweetening agents and preservatives in tobacco essence
  • Method for simultaneously determining sweetening agents and preservatives in tobacco essence

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A method for simultaneous determination of sweeteners and preservatives in tobacco essence (water-soluble sample), comprising the following steps:

[0028] 1) Sample pretreatment

[0029] Accurately weigh 0.1232g of the sample into a 50mL Erlenmeyer flask with a stopper, add 50mL of water, and adjust the pH of the solution to 9.5 with NaOH, extract with high-speed homogenization (10000rpm) for 1.5min, and purify it through an OasisHLB column (activated with 3mL of methanol and 3mL of water) ( After the flow rate is <1.0mL / min), pass through a 0.45 μm polyethersulfone filter membrane, discard the first few milliliters of filtrate, and collect subsequent filtrates for testing;

[0030] 2) Prepare mixed standard solution

[0031] Mixed standard solutions with a series of concentrations were prepared using NaOH solution at pH 9.5, and the specific concentrations of the standard substances are shown in Table 1 below;

[0032] Table 1 Concentration table of mixed standard s...

Embodiment 2

[0053] A method for the simultaneous determination of sweeteners and preservatives in tobacco essence (water-insoluble samples), comprising the following steps:

[0054] 1) Sample pretreatment

[0055] Accurately weigh 0.1009g of the sample into a 50mL Erlenmeyer flask with a stopper, add 50mL of 1:3 (v / v) methanol aqueous solution, adjust the pH value of the solution to 9.5 with NaOH, and extract with high-speed homogenization (10000rpm) for 1.5min. Move the solution to a high-speed centrifuge (16,000 rpm) for separation for 1 min, take the supernatant and pass it through an OasisHLB column (activated with 3 mL of methanol and 3 mL of water) for purification (flow rate < 1.0 mL / min), pass through a 0.22 μm nylon filter membrane, and discard For the first few milliliters of filtrate, collect the subsequent filtrate for testing;

[0056] 2) The preparation of the mixed standard solution and the standard curve making are the same as in Example 1;

[0057] 3) Sample analysis an...

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Abstract

The invention discloses a method for simultaneously determining sweetening agents and preservatives in tobacco essence, and belongs to the technical field of chemical component detection of auxiliary materials for tobaccos. The method comprises the following steps that 1, a sample to be determined is diluted, the pH value of a solution is regulated to be 9-10, extraction is performed, extraction liquid is purified through an Oasis HLB column, and the purified extraction liquid is filtered for standby application; 2, filtrate is taken to be subjected to ion chromatographic analysis, and the content of the sweetening agents and the preservatives in the sample to be determined is calculated by contrasting a standard curve. According to the method, impurities disturbing determination in the essence are purified and removed in a classifying mode according to the physical and chemical properties of different types of the tobacco essence, one-time sample feeding is performed on the three sweetening agents (sodium cyclamate, acesulfame and saccharin sodium) and the two preservatives (sorbic acid and benzoic acid) through an AS17C analytical column and an electrical conductivity detector, and separation and determination are simultaneously performed. Compared with an industrially recommended determination method, the method has the advantages of being wide in linear range, low in quantitation limit, little in sampling quantity, high in determination efficiency and the like.

Description

technical field [0001] The invention relates to a method for simultaneously measuring sweeteners and preservatives in tobacco essence, and belongs to the technical field of chemical component detection of tobacco auxiliary materials. Background technique [0002] In 2011, the Ministry of Health and the Ministry of Agriculture published a list of 151 substances illegally added to food and feed based on the problems found in risk monitoring and supervision and spot checks, including 47 kinds of "non-edible substances illegally added" in food , 22 kinds of "food additives that are prone to abuse" and 82 kinds of "drugs and substances that are prohibited from being eaten in feed, animal drinking water, and livestock and poultry aquaculture". Sorbic acid, cyclamate, benzoic acid, acesulfame potassium and sodium saccharin are "food additives easily abused" in the list of 151 illegal additives, and GB2760-2014 "Usage Standards for Food Additives" has strict regulations on their add...

Claims

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Application Information

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IPC IPC(8): G01N30/96
CPCG01N30/96G01N2030/965
Inventor 王颖边照阳刘岩顺杨飞李中皓刘珊珊范子彦邓慧敏张艳革唐纲岭
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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