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HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing content of chromium in paper for cigarette

A quantitative analysis, chromium content technology, applied in the direction of analysis of materials, measurement devices, material separation, etc., can solve the problem that the key analysis conditions and interference conditions are far apart, and achieve high sensitivity, low detection limit, good repeatability Effect

Active Publication Date: 2014-04-16
CHINA TOBACCO GUANGDONG IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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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  • HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing content of chromium in paper for cigarette
  • HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing content of chromium in paper for cigarette
  • HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing content of chromium in paper for cigarette

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0059] (1) Instruments and reagents

[0060] Agilent 7700x inductively coupled plasma mass spectrometer (Agilent, USA); 1200 high-performance liquid chromatography (Agilent, USA); SIGMA 3-18K high-speed centrifuge (SIGMA, Germany); SHZ-82 water bath constant temperature oscillator ( Jintan Guowang Experimental Instrument Factory); Milli-Q Integral ultrapure water system (Millipore, USA).

[0061] Cr (Ⅲ) single element standard stock solution (GBW08614, 1000 mg / L, National Research Center for Standard Materials); Cr (Ⅵ) single element standard stock solution (GBW(E) 080257, 100 mg / L, National Standard Material Research Center ); HNO 3 (UP grade); Ammonia (UPLC grade); Mobile phase NH 4 NO 3 by HNO 3 Prepared by mixing with ammonia water; tuning solution (Ce, Co, Li, Mg, Tl, Y, all 1 μg / L, Agilent, USA).

[0062] (2) Instrument conditions

[0063] The high-performance liquid chromatography and the inductively coupled plasma mass spectrometer are connected by PEEK tubes, an...

Embodiment 2

[0090] (1) The apparatus and reagents are the same as in Example 1.

[0091] (2) The main instrument parameter conditions of the experiment are shown in Table 3 and Table 4:

[0092] Table 3 HPLC conditions

[0093]

[0094] Table 4 ICP-MS working conditions

[0095]

[0096] (3) Sample pretreatment

[0097] Cut the cigarette paper samples 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 20 mL of 30 mmol / L NaOH solution into the quantitative bottle, tightly close the bottle cap and place it in an orbital shaker at 120 r / min The extraction rate was 1.5 h, and it was left to stand for 10 min after completion. 3 mL of the extract was filtered through a 0.45 μm water-based filter membrane, the initial 1 mL of filtrate was discarded, and the subsequent 0.8 mL of filtrate was collected to obtain the initial filtrate. Use 0.2 mol / L HCl solution to adjust the initial pH val...

Embodiment 3

[0100] (1) The apparatus and reagents are the same as in Example 1.

[0101] (2) The main instrument parameters of the experiment are the same as those in Example 1.

[0102] Cut the cigarette paper samples 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 pH value of the initial filtrate to 7.0, which is the HPLC-ICP / MS analysis solution for detecting the content of hexavalent chromium.

[0103] Others are the same as embodiment 1. The expe...

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Abstract

The invention relates to the technical field of tobacco detection and analysis and discloses an HPLC (High Performance Liquid Chromatography)-ICP (Inductively Coupled Plasma) method for quantitatively analyzing the content of chromium in a paper for a cigarette. The content of the chromium in the paper for the cigarette includes the content of hexavalent chromium and the content of trivalent chromium. With the adoption of the HPLC-ICP method, a sample is pretreated to obtain a sampling liquid, sampling analysis is directly carried out on the sampling liquid, the interference of a mass spectra and the interference of the trivalent chromium contained in the paper for the cigarette to the detection analysis of the hexavalent chromium are effectively eliminated, a high performance liquid chromatography and an inductively coupled plasma mass spectrometry condition are accurately limited, and the content of the hexavalent chromium is accurately analyzed; the pretreatment and complexation are carried out on the sample to obtain the sampling liquid, and the contents of the trivalent chromium and the hexavalent chromium in the paper for the cigarette are quantitatively analyzed and determined. The HPLC-ICP method has the advantages of low detection limit, high sensitivity, high recovery, good repeatability, short analysis time and the like and provides a strong technical base for determining the trivalent chromium and the hexavalent chromium in the mass samples.

Description

technical field [0001] The invention relates to the technical field of tobacco detection, in particular to an HPLC-ICP / MS method for quantitative analysis of chromium content in cigarette paper. Background technique [0002] At present, the most effective method for analyzing trace 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 ICP-MS To measure. 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 properties as hexavalent chrom...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/88
Inventor 古君平胡静施文庄韩冰
Owner CHINA TOBACCO GUANGDONG IND
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