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Method of detecting trivalent chromium in health food

A health food and detection method technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of not considering the conversion of hexavalent chromium to trivalent chromium, inaccurate detection results, etc.

Inactive Publication Date: 2018-01-12
广东中测食品化妆品安全评价中心有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the prior art, high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP / MS) is commonly used to detect chromium. For example, Chinese patent CN103728388A discloses a HPLC-ICP method for quantitative analysis of chromium content in cigarette paper. / MS method, Chinese patent CN101566603A discloses a method for detecting Cr(III) and Cr(VI) in cosmetics by HPLC-ICP / MS combined technology, Hu Yujun, etc. disclose high-performance liquid chromatography (HPLC) and inductively coupled plasma Method for simultaneous determination of trivalent chromium and hexavalent chromium in dairy products using mass spectrometer (ICP-MS) (see "HPLC-ICP-MS Determination of Trivalent Chromium and Hexavalent Chromium in Dairy Products", Hu Yujun et al., Modern Food Science and Technology, [J], 2014 (4): 301~305), but these methods do not consider the problem that hexavalent chromium is converted into trivalent chromium, and there is the problem of inaccurate detection results

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  • Method of detecting trivalent chromium in health food
  • Method of detecting trivalent chromium in health food
  • Method of detecting trivalent chromium in health food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] Weigh Cr (Ⅲ) single element standard stock solution (GBW08614, 1000mg / L, National Standard Material Research Center), with nitric acid-EDTA disodium buffer solution (pH value is 7.1, 50mmol / L nitric acid+0.6mmol / L EDTA) to prepare samples to be tested with concentrations of 0, 3, 9, 18, 50, and 100 μg / L, filter through a 0.22 μm organic filter membrane, and perform liquid chromatography and inductively coupled plasma mass spectrometry analysis;

[0140] The chromatographic condition of described liquid chromatography is:

[0141] Analytical column: cation exchange column;

[0142] Mobile phase: nitric acid-EDTA disodium buffer solution, the pH value of the nitric acid-EDTA disodium buffer solution is 7.1;

[0143] Flow rate: 0.5mL / min;

[0144] Elution method: isocratic elution;

[0145] Injection volume: 10μL;

[0146] Detection time: 2min;

[0147] The conditions for inductively coupled plasma mass spectrometry are:

[0148] Atomizer: glass concentric atomizer;...

Embodiment 2

[0159] Take 0.0503 g of chromium picolinate tablets and pulverize them, add 2 mL of 10% HCl solution and 0.1 mol / L hydrochloric acid into the Erlenmeyer flask, sonicate at 80°C for 30 min, cool to room temperature, and under the condition of pH 7.1 Complexation reaction with mL nitric acid-ethylenediaminetetraacetic disodium buffer solution (pH value 7.1, 50mmol / L nitric acid + 0.6mmol / L EDTA) in a 50°C water bath for 1h, after cooling to room temperature, Disodium amine tetraacetate buffer solution (pH value is 7.1, 50mmol / L nitric acid + 0.6mmol / L EDTA) was diluted to the concentration range of the standard curve, and finally filtered through a 0.22μm organic filter membrane for liquid chromatography and inductance Coupled plasma-mass spectrometry analysis.

[0160] Using the same liquid chromatography and inductively coupled plasma mass spectrometry conditions as in Example 1 to detect the liquid to be tested, the obtained liquid chromatogram is as follows image 3 as show...

Embodiment 3

[0162] Using the same steps as in Example 2, the only difference is that 0.0503 g of the chromium picolinate tablet is replaced by 0.0510 g. The obtained phase chromatogram is as Figure 4 as shown, Figure 4 Middle 1 is the Cr(Ⅲ) peak, and the area of ​​peak 1 is 829633. The concentration of Cr(Ⅲ) in the health food test solution calculated by the external standard method and the standard equation is 81.704μg / L, and the content of Cr(Ⅲ) in the sample is calculated to be 1602.0mg / kg. The calculation results are based on the repeatability conditions. The arithmetic mean of the results obtained for two independent determinations is represented with a relative standard deviation of 2.0%.

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Abstract

The invention provides a method of detecting trivalent chromium in health food, and belongs to the technical field of food detection. According to the method provided by the invention, hexavalent chromium is prevented from being converted into trivalent chromium to generate interference by limiting the pH value of a complexing reaction to 7.1; moreover, separation and measurement of trivalent chromium in health food are realized by accurately limiting the liquid chromatography conditions and the inductively coupled plasma-mass spectrometry conditions. Data of embodiments indicate that the separation and measurement of trivalent chromium in health food are realized in the invention, and the standard deviation between the peak area and the retention time of inductively coupled plasma-mass spectrometry is relatively low; moreover, the linear correlation coefficient of a standard equation is as high as 0.9997, thereby ensuring relatively high accuracy and sensitivity.

Description

technical field [0001] The invention relates to the technical field of food detection, in particular to a method for detecting trivalent chromium in health food. Background technique [0002] Chromium is an element that widely exists in nature, mainly distributed in rocks, soil, atmosphere, water and organisms. Chromium is an element with dual effects. It is not only one of the essential trace elements for the human body, but it can also lead to poisoning and even death when the intake is too high. [0003] The common valence states of chromium compounds are trivalent and hexavalent, and trivalent chromium and hexavalent chromium compounds can be transformed into each other. In water, hexavalent chromium is generally expressed as CrO 2 -4 、HCr 2 o -7 、Cr 2 o 2 -7 There are three anion forms, which are affected by factors such as water pH, temperature, redox substances, organic matter, etc. The toxicity of chromium is related to its existing valence state. In the pri...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 秦俊莲孔令梁陈智勇庞璐杨逸菲黄伟业
Owner 广东中测食品化妆品安全评价中心有限公司