Method for measuring residual maleic hydrazide in tobacco or tobacco product

A technology for maleic hydrazide and tobacco products, which is applied in the field of determination of maleic hydrazide residues, can solve problems such as different purification methods and complex extracts, and achieve the effects of improved accuracy, high sensitivity, and easy popularization and application

Active Publication Date: 2010-11-03
ZHENGZHOU TOBACCO RES INST OF CNTC
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Problems solved by technology

Due to the different matrices of potato samples and tobacco samples, and the extracts of tobacco samples are more complex, and the purification methods are also very different, so the determination methods reported in these two literatures are difficult to apply in tobacco and tobacco products, and new methods need to be developed. Detection method of maleic hydrazide in tobacco and tobacco products

Method used

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  • Method for measuring residual maleic hydrazide in tobacco or tobacco product
  • Method for measuring residual maleic hydrazide in tobacco or tobacco product
  • Method for measuring residual maleic hydrazide in tobacco or tobacco product

Examples

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Effect test

Embodiment 1

[0029] 1. Instruments and reagents

[0030] Maleic hydrazide standard (Augsburg, Germany); HPLC grade glacial acetic acid (TEDIA, USA); ammonium acetate (TEDIA, USA); PPt grade ultrapure water;

[0031] Agilent1200 high performance liquid chromatography, equipped with VWD ultraviolet detector; pure water meter (MILLIPORE, USA); PHS-3C precision pH meter (Shanghai Leici Instrument Factory); ZNHW electric heating mantle (Henan Yuhua Instrument Co., Ltd.), VarianMicrosorb -MV100-5C18 (250*4.6mm) chromatographic column; SUPLCOC18 solid phase extraction cartridge.

[0032] 2. Determination steps:

[0033] 1) Sample pretreatment:

[0034] Weigh 3.0-5.0g of tobacco powder sample A, put it in a 250mL ground-mouthed round-bottom flask, add 50.00mL of 1mol / L hydrochloric acid, heat to 180°C and reflux for 1 hour, take it down and cool to room temperature, filter with double-layer filter paper, Take 2.00mL of the filtrate and add it to a C18 solid-phase extraction cartridge for purifi...

Embodiment 2

[0046] The assay method of the present embodiment is basically the same as that of Example 1, the difference being that the temperature of the extraction is 200°C, the extraction time is 1.5 hours, the concentration of the hydrochloric acid solution used in the extraction is 2mol / L, and the concentration of the sodium hydroxide solution during elution is 0.15mol / L; the mobile phase was adjusted to pH 5.2 with ammonium acetate, and the flow rate was 0.8mL / min. Another tobacco leaf sample B was selected, and the residual amount of maleic hydrazide in sample B was measured to be 11.7 μg / g.

Embodiment 3

[0048] The assay method of the present embodiment is basically the same as that of Example 1, the difference being that the temperature of the extraction is 190°C, the extraction time is 2 hours, the concentration of the hydrochloric acid solution used in the extraction is 3mol / L, and the concentration of the sodium hydroxide solution during elution is 0.2mol / L; the mobile phase was adjusted to pH 5.4 with ammonium acetate, and the flow rate was 0.9mL / min. Another tobacco leaf sample C was selected, and the residual amount of maleic hydrazide in sample C was measured to be 140.4 μg / g.

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Abstract

The invention discloses a method for measuring residual maleic hydrazide in a tobacco or a tobacco product, which mainly comprises the following steps of: heating a sample for reflux extraction by using hydrochloric acid solution; performing purification by using a small C18 solid phase extraction column; performing eluation by using sodium hydroxide solution to obtain sample solution; and measuring the residual maleic hydrazide in the sample by using a high-efficiency liquid chromatography and adopting an external standard method. The method for measuring the residual maleic hydrazide in thetobacco or the tobacco product adopts a sample pretreatment method combining liquid-phase extraction and solid-phase extraction to not only shorten the pretreatment time of the sample but also improve the measuring accuracy; the measuring method has the advantages of high sensibility, high repeatability and wide detection range, the average recovery rate is 99 percent, and the detection range is between 0.1 and 80 mu g / ml; besides, the method is simple and quick to operate, has high degree of automation, and is easy for popularization and application.

Description

technical field [0001] The invention relates to a method for determining the residual amount of maleic hydrazide in tobacco or tobacco products, and belongs to the technical field of trace analysis. Background technique [0002] Tobacco is a smoking food, and its pesticide residue problem has become an important part of smoking safety issues. The pesticide residue index of tobacco and tobacco products is an important content in the quality control of tobacco products in various countries, and has become an important part of tobacco leaf evaluation and selection in the international market. It is an important factor in the purchase of tobacco and an important content of commodity inspection in the international trade of tobacco. The pesticide maleic hydrazide is an important indicator for the detection of tobacco pesticide residues. In 2008, the Agricultural Chemicals Committee (ACAC) of the International Tobacco Scientific Research Cooperation Center (CORESTA) proposed 136 p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/36G01N30/06
Inventor 唐纲岭张洪非边照阳胡清源李中皓陈再根朱凤鹏侯宏卫陈欢刘楠姜兴益
Owner ZHENGZHOU TOBACCO RES INST OF CNTC
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