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Method for measuring phthalate ester content of tipping paper for tobaccos

A technology of phthalic acid and ester compounds, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of reducing errors, improving sensitivity, and good repeatability

Inactive Publication Date: 2012-01-25
HONGYUN HONGHE TOBACCO (GRP) CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no report on the detection of phthalates in cigarette tipping paper by gas chromatography-mass spectrometry. Cigarette tipping paper, as an important cigarette product material, has an important impact on the quality and safety of cigarette products. Therefore, from the perspective of the safety and sensory quality of cigarette materials, the analysis of the content of phthalates in cigarette tipping paper is of great significance for the correct evaluation and strict control of product safety.

Method used

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  • Method for measuring phthalate ester content of tipping paper for tobaccos
  • Method for measuring phthalate ester content of tipping paper for tobaccos
  • Method for measuring phthalate ester content of tipping paper for tobaccos

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Embodiment 1

[0043] Determination of the content of phthalates in cigarette tipping paper (the determination process is as follows figure 1 shown) 1. Preparation of internal standard extract:

[0044] (1) Preparation of internal standard stock solution Ⅰ: Accurately weigh 250 mg benzyl benzoate into a 100 mL volumetric flask, dilute to the mark with ethanol and mix well to obtain internal standard stock solution Ⅰ with a concentration of 2.5 mg / mL ; Store the internal standard stock solution Ⅰ in a sealed refrigerator at 4°C, and the validity period is 3 months;

[0045] (2) Preparation of internal standard stock solution II: Accurately pipette 1 mL of internal standard stock solution I into a 50 mL volumetric flask, dilute to the mark with ethanol and shake well to obtain internal standard solution II with a concentration of 50 μg / mL ;The internal standard stock solution II needs to be prepared immediately;

[0046] (3) Preparation of internal standard extract: accurately pipette 10 mL ...

Embodiment 2

[0074] 1. Preparation of sample solution: Accurately cut 20 cm×4 cm cigarette tipping paper, then cut it into fragments not larger than 1 cm×1 cm for extraction, then put it into a 50 mL conical flask, add 30 mL containing The extract of the internal standard was ultrasonically extracted for 30 min, left to stand still, and the supernatant was taken to pass through a 0.45 μm organic filter membrane, and the obtained sample solution was used for gas chromatography-mass spectrometry analysis;

[0075] 2, adopt the chromatographic mass spectrometry condition analysis sample solution of embodiment 1;

[0076] 3, will record 7 kinds of phthalates and the chromatographic peak area ratio of internal standard, substitute into the standard curve that embodiment 1 draws, obtain the content of phthalates in the sample, calculation method is the same as implementing The calculation method of Example 1, the specific calculation results are shown in Table 4.

[0077] Table 4 Test results o...

Embodiment 3

[0081] The present embodiment is as follows to the detection method of the repeatability of the inventive method and the standard addition recovery rate:

[0082] Add each phthalate standard sample of 3 different concentrations of high, middle and low respectively in the sample, measure 5 times respectively for each sample, the chromatography mass spectrometry analysis condition is the same as the chromatography mass spectrometry analysis condition of embodiment 1, calculate this method according to the analysis result The recovery rate of phthalates in cigarette tipping paper and the relative standard deviation of the value measured after the standard addition, the results are shown in Table 5:

[0083] Table 5 The recovery rate and standard deviation of phthalates in cigarette tipping paper

[0084] name Recovery rate(%) RSD(%) Dimethyl phthalate (DMP) 95.2 3.4 Diethyl phthalate (DEP) 97.3 4.1 Diisobutyl phthalate (DIBP) 103.2 4.8 Di-n...

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Abstract

The invention discloses a method for measuring the phthalate ester content of tipping paper for tobaccos. The method comprises the steps of: preparation of internal standard extract liquor, standard working solution and sample solution, gas chromatography-mass spectrography, calculation of measurement results and the like. The improved and optimized measurement method has the advantages of operation simplicity and accuracy, high sensitivity, high recovery rate, high repeatability and the like. Errors caused by pretreatment or apparatus precision and the like are effectively reduced by utilizing an internal standard quantity. Under adopted chromatographic conditions, seven target compounds and internal standard chromatographic peaks have relatively higher degrees of separation, relatively higher linear correlation and the detection limit of 0.01 to 0.03 mu g per centimeter spare. By the method, a standard recovery rate is 94 to 106 percent and an average relative standard deviation is 3.4 to 4.8.

Description

technical field [0001] The invention belongs to the technical field of physical and chemical inspection of cigarette materials, and in particular relates to a method for measuring the content of phthalate compounds in tipping paper for cigarettes. Background technique [0002] Cigarette tipping paper is an important material in the cigarette production process. It is a special paper for connecting filters and cigarettes, commonly known as tipping paper. Ink printing materials are widely used in the cigarette production process, adding phthalate compounds in ink can improve the processing performance of ink. [0003] Phthalate is a general term for a class of compounds. It is a product obtained by the reaction of phthalic anhydride and alcohol. It is odorless or slightly smelly. It is mainly used as a plasticizer. Phthalates are a class of environmental hormones. Can lead to endocrine disorders, reproductive dysfunction and so on. Among the phthalates, 7 have been listed b...

Claims

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Application Information

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IPC IPC(8): B01D11/04G01N30/06G01N30/72
Inventor 范多青史小波王庆华李响丽李世杰郭丽娟缪艳霞
Owner HONGYUN HONGHE TOBACCO (GRP) CO LTD
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