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Method for detecting musk xylene in tobacco additive

A technology for xylene musk and tobacco additives, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of public reports on the detection method of xylene musk in tobacco additives that have not been seen, and achieve high sensitivity and accurate determination methods Effect

Inactive Publication Date: 2012-07-18
YUNNAN RES INST OF TOBACCO SCI
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Problems solved by technology

[0004] After literature search, there is no public report on the detection method of xylene musk in tobacco additives

Method used

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  • Method for detecting musk xylene in tobacco additive
  • Method for detecting musk xylene in tobacco additive
  • Method for detecting musk xylene in tobacco additive

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Embodiment Construction

[0031] The present invention is described in further detail below:

[0032] 1. Experimental part

[0033] 1.1 Instruments and reagents

[0034] Instruments and equipment: PE-Clarus600T mass spectrometer (PE in the United States), HP-5MS (0.25μm×250μm×30m) chromatographic column (Agilent in the United States), XP504 analytical balance (Mettler in Switzerland), SHZ-82 constant temperature oscillator ( Changzhou Guohua), SK5200H ultrasonic oscillator (Shanghai Kedao), LG10-2.4A high-speed centrifuge (Beijing Medical), separating funnel, pipette, and other common experimental glassware.

[0035] Reagents: cyclohexane, toluene, chloroform, D 15- musk xylene standard, musk xylene standard, anhydrous sodium sulfate, ultrapure water (resistivity 18.2MΩ).

[0036] 1.2 Preparation of standard solution

[0037] Weigh 0.1 g (accurate to 0.001 g) of musk xylene standard substance in a 100 mL volumetric flask, dissolve it with cyclohexane and adjust the volume to the mark, prepare a 1 m...

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Abstract

The invention relates to a method for detecting musk xylene in a tobacco additive and belongs to the technical field of detection of tobacco additives. The method comprises the following steps of: weighing 1.0g of tobacco additive and putting into a 50mL conical flask with a plug, adding 10mL of ultrapure water of which electrical resistivity is 18.2 M Omega and dispersing a sample, adding 0.3mL of D15-musk xylene interior label solution with the concentration of 1mu g / mL, and 10mL of cyclohexane, oscillating and extracting at the temperature of 25 DEG C for 10 minutes, centrifuging a mixed solution at rotation speed of 4,000r / min by a centrifugal machine for 10 minutes, extracting an upper-layer organic phase, adding 10mL of chromatographically pure cyclohexane into a water phase of which the upper-layer organic phase is extracted, performing secondary extraction under the same operation conditions, centrifuging, and extracting an upper-layer organic phase; and mixing the organic phases extracted twice, drying by using anhydrous sodium sulfate, and metering the volume to ensure that the volume is 1mL for gas chromatography-mass spectrometer (GC-MC) determination. The method has the advantages of high sensitivity and capacity of effectively determining the content of musk xylene in the tobacco additive, and can determine the content of the musk xylene accurately and quickly, and is suitable for monitoring and self-inspection work of the highly-concerned musk xylene in the tobacco additive.

Description

Technical field: [0001] The invention relates to a method for detecting xylene musk in tobacco additives, and belongs to the technical field of detection of tobacco additives. Background technique: [0002] Musk xylene is a synthetic nitroaromatic musk compound with the chemical name 2,4,6-trinitro-1,3-dimethyl-5-tert-butylbenzene. It has the characteristics of special fragrance and long-lasting fragrance, and is often used as a fixative for cosmetics and soap essences [1] . However, due to reports that musk xylene can cause cancer in mice [2] , and as a highly persistent and highly bioaccumulative substance, it has been listed as a substance of very high concern by the European Chemicals Agency [3，4] ; In July 2009, the International Daily Chemical Fragrance Association also announced the complete ban on p-xylene musk [5] , the domestic tobacco industry also explicitly prohibits the use of musk xylene in tobacco additives. [0003] At present, domestic and foreign rese...

Claims

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Application Information

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IPC IPC(8): G01N30/88G01N30/06
Inventor 陈建华耿永勤李雪梅缪明明徐济仓缪恩铭杨叶昆魏玉玲周岚
Owner YUNNAN RES INST OF TOBACCO SCI
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