HPLC(high performance liquid chromatography)/MS(mass spectrometry)/MS method suitable for quantitatively detecting perfluoro caprylic acid in animal-origin food

An animal-derived, quantitative detection technology, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of inability to effectively extract PFOA and interfere with the detection and analysis of PFOA, so as to shorten the detection time, reduce detection costs, and reduce purification The effect of steps

Inactive Publication Date: 2015-07-01
SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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Problems solved by technology

However, due to the interference of organic impurities such as fat and protein in animal foods, organic solvents such as methanol cannot ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Sample purification treatment by sulfonation method: 5 grams of freeze-dried fish meat samples were weighed and placed in a beaker, and 5 ml of 60% sulfuric acid solution was slowly dripped in with a dropper. After sulfonating the acid solution at 50°C for 25 minutes, the mixture of the sample and sulfuric acid was slowly transferred to a beaker filled with 30ml of supersaturated sodium peroxide solution.

[0020] (2) Organic solvent extraction: Add 50 mL of acetonitrile solvent into a beaker containing the mixed solution, then transfer to a separatory funnel for vibration extraction for 10 minutes, then add excess sodium chloride and shake for 2 minutes, and separate the upper organic layer solvent.

[0021] (3) The separated organic solvent was concentrated to near-dryness in a water bath at 40°C, then dissolved in methanol and transferred to an injection bottle to make up to 0.2ml, and finally injected to HPLC-MS / MS for detection and analysis.

[0022] (4) HPLC-M...

Embodiment 2

[0024] (1) Sample purification treatment by sulfonation method: Weigh 5 grams of freeze-dried ham sausage sample and place it in a beaker, slowly drop into 5 ml of 70% sulfuric acid solution with a dropper. After sulfonating the acid solution at 50°C for 30 minutes, the mixture of the sample and sulfuric acid was slowly transferred to a beaker filled with 30ml of supersaturated sodium peroxide solution.

[0025] (2) Organic solvent extraction: Add 50 mL of acetone solvent into a beaker containing the mixed solution, then transfer to a separatory funnel for vibration extraction for 10 minutes, then add excess sodium chloride and shake for 2 minutes, and separate the upper organic layer solvent.

[0026] (3) The separated organic solvent was concentrated to near-dryness in a water bath at 40°C, then dissolved in methanol and transferred to an injection bottle to make up to 0.2ml, and finally injected to HPLC-MS / MS for detection and analysis.

[0027] (4) HPLC-MS / MS chromatograph...

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Abstract

The invention relates to a perfluoro caprylic acid detecting method in the field of environmental analytical chemistry, in particular to a HPLC (high performance liquid chromatography)/MS(mass spectrometry)/MS method suitable for quantitatively detecting perfluoro caprylic acid in animal-origin food. In order to solve the problems that the perfluoro caprylic acid cannot be effectively extracted due to components of fat, proteins and the like in the animal food and the quantitative detection is severely interfered by a complex sample substrate, the HPLC-MS/MS method for quantitatively detecting perfluoro caprylic acid in animal-origin food is established by performing sulphonation-process purification on an animal-origin food sample by utilizing the chemical stability of the perfluoro caprylic acid to concentrated sulfuric acid, and effectively extracting a target compound by adopting a salting-out and layering method. Compared with the prior art, impurities of fat, proteins and like in a sample are digested by sulfuric acid sulphonation, the recovery rate is increased, the substrate interferences are reduced, the detection time is shortened, and the detection cost is reduced. The HPLC-MS/MS method is very suitable for detecting a large number of samples.

Description

technical field [0001] The present invention relates to a method suitable for rapid and quantitative detection of perfluorooctanoic acid in animal-derived foods, in particular to an HPLC-MS / MS method for rapid quantitative detection of perfluorooctanoic acid in animal-derived foods by using sulfonation method purification and salting-out layering pretreatment method. Background technique [0002] Due to its excellent properties such as high thermal stability and high surface activity, perfluorooctanoic acid (PFOA) is widely used in electronics industry, electroplating and other industries, as well as cosmetics, daily washing and other civilian products. According to statistics, the total production of PFOA in the world during 1951-2004 was about 3600-5700 tons, of which about 400-700 tons of PFOA were discharged into the environment. Due to its hydrophobic and oleophobic characteristics, unlike general lipophilic organic pollutants, PFOA does not accumulate in adipose tissu...

Claims

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Application Information

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IPC IPC(8): G01N30/02
Inventor 魏东洋贺涛魏良良
Owner SOUTH CHINA INST OF ENVIRONMENTAL SCI MEP
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