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Method for measuring phthalates in flavors and fragrances for tobaccos

A technology of phthalates and tobacco flavors, applied in the field of tobacco flavors and fragrances (liquid field, can solve the problems of no impurity removal step, obvious matrix effect, pollution of analytical column and ion source, etc.

Active Publication Date: 2018-10-19
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is a recommended method for the determination of tobacco flavor in the tobacco industry, but this method uses ethanol to directly dilute the sample, uses GC-MS for measurement, and has no impurity removal steps, so there are many problems in use
On the one hand, many flavors or spices are insoluble in ethanol (such as some extracts), and on the other hand, the flavor components are complex, and direct injection will pollute the analytical column and ion source, and the matrix effect is obvious

Method used

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  • Method for measuring phthalates in flavors and fragrances for tobaccos
  • Method for measuring phthalates in flavors and fragrances for tobaccos
  • Method for measuring phthalates in flavors and fragrances for tobaccos

Examples

Experimental program
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Embodiment

[0049] Example: Determination of phthalates in tobacco flavor and fragrance samples.

[0050] (1) Pre-processing

[0051] Weigh 0.3-0.6g of flavor and fragrance samples into a 25 mL Erlenmeyer flask with a stopper, accurate to 0.0001 g, add 7-15 mL of ethanol aqueous solution (volume ratio 1:1), and then add 250 µL of internal standard solution (solvent is ethanol, Concentration is 0.1 mg / mL), ultrasonic extraction for 30min, take 2mL initial extraction solution into 15mL glass centrifuge tube, add 5mL n-hexane / ethyl acetate / isopropanol solution (volume ratio is 3:1:1), at 2000 Vortex and oscillate at rpm for 5 min, then centrifuge at 4000 rpm for 5 min, and take the supernatant for testing.

[0052] (2) Blank experiment

[0053] Repeat step (1) without adding sample.

[0054] (3) Instrument analysis

[0055] It was measured by GC-MS, and the measurement conditions were as follows.

[0056] Gas chromatography conditions:

[0057] Column stationary phase: 5% phenyl / 95% me...

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Abstract

The invention discloses a method for measuring phthalates (PAEs) in flavors and fragrances for tobaccos. The method comprises the following steps: dispersing and initially extracting samples with an aqueous ethanol solution at a certain concentration; then using a mixed solvent of n-hexane / ethyl acetate / isopropanol at a certain ratio for liquid-liquid extraction of an initial extract; directly sampling supernatant for analysis after layering through liquid-liquid extraction. The method provided by the invention can disperse most flavor and fragrance samples well in the initial extraction step,and uses the mixed solvent of n-hexane / ethyl acetate / isopropanol for the liquid-liquid extraction of the initial extract to not only purify the initial extract, but also make a recovery rate of 18 PAEs reach 90% or higher. The method uses fewer glass instruments, uses an internal standard method to further simplify a solution transfer step and greatly reduce probability of contamination during pretreatment, and is suitable for measuring mass samples.

Description

technical field [0001] The invention belongs to the field of physical and chemical analysis of harmful components of tobacco additives, and is suitable for the determination of phthalates in tobacco flavors and fragrances (liquid, paste and milk). Background technique [0002] Tobacco flavor is a kind of food flavor. Adding flavors in the process of making cigarettes can neutralize, correct, or change the taste and mouthfeel of tobacco to some extent to achieve a pleasant effect. However, tobacco flavors are not only used for flavoring shredded tobacco, but are also used on cigarette packaging materials (such as cigarette paper, filter rods, etc.) to meet the olfactory needs of consumers. It can be said that when consumers consume cigarette products, they have a very large chance of being directly exposed to tobacco flavors. At present, the safety and hygiene requirements for tobacco flavors mainly refer to food flavors. [0003] Phthalates (PAEs) are one of the controlle...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 王颖杨飞邓惠敏刘珊珊唐纲岭边照阳张威柯玮范子彦李中皓
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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