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Kit for detecting perchlorate ions in food, and detection method thereof

A technology of perchlorate and determination method, which is applied in the field of physical and chemical analysis of chemical substances, can solve the problems of single bottled water of the detection object, difficult quantitative analysis, and has not yet been seen, and achieves high sensitivity, high selectivity, good sensitivity and precision. degree of effect

Active Publication Date: 2014-08-27
INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the poor reproducibility of this technique makes quantitative analysis difficult
There are very few domestic and foreign reports on liquid chromatography-mass spectrometry / mass spectrometry detection methods for perchlorate ions in food. The detection objects are mainly a single bottled water, milk or milk powder matrix. Liquid chromatography-mass spectrometry / mass spectrometry detection method and system for perchlorate ions in foods such as grains, aquatic products, and animal tissues

Method used

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  • Kit for detecting perchlorate ions in food, and detection method thereof
  • Kit for detecting perchlorate ions in food, and detection method thereof
  • Kit for detecting perchlorate ions in food, and detection method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0121] Embodiment 1: a kind of test kit for detecting perchlorate ion in food of the present invention

[0122] A kind of test kit for detecting perchlorate ion in food of the present embodiment comprises perchlorate standard solution, 18 O marks perchlorate solution, acetic acid solution, acetonitrile, ammonium acetate solution and solid phase extraction C 18 column. CAS No of perchlorate standard solution: 7601-89-0, purity: 100%, concentration 1000mg / L. 18 The O-marked perchlorate solution is a solution with a concentration of 100 μg / L and a purity of 90%. Its preparation can be prepared according to the method described in the above reagents and materials section. said 18 O marks the perchlorate solution as containing (Cl 18 o 4 -) solution. The acetic acid solution is composed of acetic acid and water, and the volume ratio of acetic acid to the water is 1:100. The solid phase extraction C 18 The amount of filler in the column is 200mg, 3mL.

Embodiment 2

[0123] Embodiment 2: detect the multiple reaction monitoring experiment of perchlorate ion with kit of the present invention

[0124] The liquid chromatography-mass spectrometry / mass spectrometry multiple reaction monitoring experiment was performed on perchlorate ion according to the following conditions. perchlorate standard solution and 18 O-marked perchlorate solutions are all used solutions, and their configuration can be found in the above reagents and materials.

[0125] Liquid chromatography conditions:

[0126] a) Column: IC-Pak TM Anion HR column, 6μm, 4.6mm×75mm (inner diameter) or equivalent;

[0127] b) Mobile phase: acetonitrile + 0.1mol / L ammonium acetate solution = (60+40, V 1 / V 2 );

[0128] c) Flow rate: 700μL / min;

[0129] d) Column temperature: 40°C;

[0130] e) Injection volume: 10 μL;

[0131] Mass Spectrometry Conditions:

[0132] a) Ion source: electrospray ion source (ESI);

[0133] b) Scanning mode: negative ion scanning;

[0134] c) Mon...

Embodiment 3

[0144] Embodiment 3: the condition optimization experiment of detection method of the present invention

[0145] 1. Selection of extraction solvent

[0146] Perchlorate has high solubility and low adsorption, most of which are easily soluble in water. In this example, 1% acetic acid solution and water were respectively used as extraction solvents in the extraction test, and it was found that there was no difference in the solvent addition test, but after the samples (milk powder was used as an example in this example) were purified by the addition test, the results are shown in Table 1 , table 1 is the comparative result table of the influence of extraction solvent on recovery rate, and this result shows to adopt acetic acid solution, and described acetic acid solution contains acetic acid and water, and the volume percent concentration of described acetic acid solution is 1%, selects this acetic acid solution as extraction The addition and recovery of solvent is better than ...

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Abstract

The invention provides a kit for detecting perchlorate ions in a food. The kit comprises a perchlorate standard solution, a <18>O labeled perchlorate ion solution, an acetic acid solution, acetonitrile, an ammonium acetate solution and a solid phase extraction C18 column. The invention also provides a method for detecting the perchlorate ions in the food. The method comprises the following steps: 1, extracting a sample; 2, purifying; and 3, carrying out accurate qualitative and quantitative treatment by adopting a reverse phase analysis process with a high separating ability and a high signal-to-noise ratio. The kit adopts the acetic acid solution as a sample extraction solvent; the adoption of the solid phase extraction column to purity realizes a good recovery rate and a good purification effect; and the kit and the method adopt a soft ionization technology to detect and an internal standard method to quantify in order to realize high selectivity, high sensitivity and wide application range, have extremely high specificity, and can be widely applied to detect the perchlorate ions in the food.

Description

technical field [0001] The invention relates to the field of physical and chemical analysis of chemical substances, in particular to a kit for detecting perchlorate ions in food and a determination method thereof. Background technique [0002] Perchlorate refers to containing perchlorate ([ClO 4 ] - ) salts, both naturally occurring and artificially synthesized. Perchlorate ion has a similar charge and ionic radius to iodide ion, and has a higher affinity for iodine ion transporter than iodine, so it can inhibit the absorption of iodine, weaken the thyroid function, cause human metabolic disorder, affect the fetus and Normal growth and development of the baby's nerve center, severe hypothyroidism in pregnant women can lead to cretinism in the fetus. Due to the high solubility and low adsorption of perchlorate, it is easy to irrigate through water sources, absorb and accumulate in plants, and finally pass it on to humans. Its pollution problem has attracted great attentio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
Inventor 吴映璇林峰邵琳智欧阳少伦姚仰勋谢敏玲
Owner INSPECTION & QUARANTINE TECH CENT OF GUANGDONG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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