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A pretreatment method for HPLC-ICP/MS analysis of chromium content in cigarette paper

A technology of chromium content and paper, which is applied in the field of pretreatment for analyzing chromium content in cigarette paper by HPLC-ICP/MS, which can solve the problems of the key analysis conditions and interference conditions being far apart.

Active Publication Date: 2015-09-30
CHINA TOBACCO GUANGDONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the key analysis conditions and interference conditions involved in instrument-based detection and analysis methods are quite different. Different tobacco companies have different detection and analysis instruments and experimental conditions, so they cannot be simply referred to.

Method used

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  • A pretreatment method for HPLC-ICP/MS analysis of chromium content in cigarette paper
  • A pretreatment method for HPLC-ICP/MS analysis of chromium content in cigarette paper
  • A pretreatment method for HPLC-ICP/MS analysis of chromium content in cigarette paper

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Experimental program
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Effect test

Embodiment 1

[0062] Treatment 1: The pretreatment method of cigarette tipping paper samples shall be carried out according to the requirements stipulated in YC / T 171-2009, and then the samples shall be cut into pieces with a size of 0.5 cm×0.5 cm. Accurately weigh 0.5 g of the pretreated sample and place it in a 15 mL plastic centrifuge tube, add 10 mL of 50 mmol / L NaOH solution into the tube, tightly close the cap of the tube and place it in a rotary shaker at 120 r / min Extract at a high rate for 2 h, and let stand for 10 min after completion. Take 3 mL of the extract and filter it through a 0.45 μm aqueous filter membrane, discard the initial 1 mL of filtrate, and collect the subsequent 1 mL of filtrate to obtain the initial filtrate. Use 0.1 mol / L HCl solution to adjust the initial pH value of the filtrate to 7.0, and then carry out complexation reaction with 10 mL of 10 mmol / L EDTA (disodium salt or dipotassium salt) solution at 80°C for 20 min. The solution is HPLC-ICP / MS analysis so...

Embodiment 2

[0065] Treatment 1: Cut the molded paper samples for cigarettes into pieces with a size of 0.5 cm×0.5 cm. Accurately weigh 1.0 g of the pretreated sample and place it in a 30 mL plastic quantitative bottle, add 15 mL of 50 mmol / L NaOH solution into the quantitative bottle, tightly close the bottle cap and place it in a rotary shaker at 150 r / min The extraction rate was 2 h, and then it was left to stand for 10 min. Take 3 mL of the extract and filter it through a 0.45 μm aqueous filter membrane, discard the initial 1 mL of filtrate, and collect the subsequent 1 mL of filtrate to obtain the initial filtrate. Use 0.1 mol / L HCl solution to adjust the initial pH value of the filtrate to 7.0, and then carry out complexation reaction with 10 mL of 10 mmol / L EDTA (disodium salt or dipotassium salt) solution at 60°C for 30 min. The solution is HPLC-ICP / MS analysis solution A.

[0066] Treatment 2: Cut the molded paper samples for cigarettes into pieces with a size of 0.5 cm×0.5 cm. ...

Embodiment 3

[0068] Treatment 1: Cut the cigarette paper samples for cigarettes into pieces with a size of 0.5 cm×0.5 cm. Accurately weigh 1.0 g of the pretreated sample and place it in a 30 mL plastic quantitative bottle, add 15 mL of 50 mmol / L NaOH solution into the quantitative bottle, tightly close the bottle cap and place it in a rotary shaker at 150 r / min The extraction rate was 2 h, and then it was left to stand for 10 min. Take 3 mL of the extract and filter it through a 0.45 μm aqueous filter membrane, discard the initial 1 mL of filtrate, and collect the subsequent 1 mL of filtrate to obtain the initial filtrate. Use 0.1 mol / L HCl solution to adjust the initial pH value of the filtrate to 7.0, and then carry out complexation reaction with 10 mL of 15 mmol / L EDTA (disodium salt or dipotassium salt) solution at 50°C for 60 min. The solution is the HPLC-ICP / MS analysis solution.

[0069] Treatment 2: Shred the cigarette paper sample into pieces of 0.5 cm×0.5 cm. Accurately weigh ...

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Abstract

The invention belongs to the technical field of tobacco analysis and detection and discloses a pretreatment method for analyzing the content of chrome in cigarette paper by HPLC-ICP / MS. The cigarette paper sample is subjected to shaking extraction by using a NaOH solution, the extraction solution is filtered by an aqueous filter membrane to obtain an initial filter solution, the pH value of the initial filter solution is adjusted by using an HCl solution, and finally the obtained filter solution is used as the analysis solution of the hexavalent chrome; or after the pH value of the initial filter solution is adjusted, the adjusted filter solution is allowed to complex with EDTA solution, and finally the complex reaction solution is used as the analysis solution of the trivalent chrome and the hexavalent chrome in the cigarette paper by HPLC-ICP / MS. The invention provides the chromatographic separation pretreatment method for the separation and measurement process of the trivalent chrome and the hexavalent chrome in the cigarette paper by using the high performance lquid chromatography (HPLC)-inductively coupled plasma mass spectrometry(ICP / MS). The pretreatment method has the advantages of convenience in operation, specific reaction and easiness in control, and provides powerful technical basis for measurement of the trivalent chrome and the hexavalent chrome in bulk samples.

Description

technical field [0001] The invention relates to the technical field of tobacco detection, in particular to a pretreatment method for HPLC-ICP / MS analysis of chromium content in cigarette paper. Background technique [0002] At present, the most effective method for analyzing trivalent chromium and hexavalent chromium is high performance liquid chromatography combined with inductively coupled plasma mass spectrometry (HPLC-ICP-MS), which uses HPLC to separate Cr(Ⅲ) and Cr(Ⅵ) into Measured in ICP-MS. Chromatographic separation in this technology mainly has the following methods: [0003] a: C8 column [0004] Since trivalent chromium and hexavalent chromium have different charging properties, the separation performance on the same column is different. In order to achieve a better separation state, when using a C8 column as a stationary phase, it is necessary to complex trivalent chromium and EDTA first, so that the trivalent chromium-EDTA complex has the same electrical pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/06
Inventor 古君平胡静施文庄韩冰
Owner CHINA TOBACCO GUANGDONG IND
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