Method for determination of residual quantity of pentachlorophenol in eggs and egg products

A pentachlorophenol and residue technology, which is applied to the extraction of pentachlorophenol residues in poultry eggs and poultry egg products, the determination of pentachlorophenol residues in poultry eggs and poultry egg products, small column enrichment purification and liquid chromatography -In the field of tandem mass spectrometry determination, it can solve the problems that the elution and elution procedures cannot achieve the ideal purification effect, it is difficult to meet the detection limit requirements of the method, and the accuracy of the detection results is affected, so as to overcome the incomplete enrichment and purification, good detection sensitivity and precision food safety and human health

Inactive Publication Date: 2018-01-26
NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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Problems solved by technology

[0004] One is that the absolute recovery rate is low. Existing literature such as the international method for sample extraction "using 5% triethylamine in acetonitrile-water solution as the extractant" is more effective for lean meat and skimmed milk, but for poultry eggs and poultry egg products , the absolute recovery rate of the extraction is very low, and it is difficult to meet the detection limit requirements of the m...

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  • Method for determination of residual quantity of pentachlorophenol in eggs and egg products
  • Method for determination of residual quantity of pentachlorophenol in eggs and egg products
  • Method for determination of residual quantity of pentachlorophenol in eggs and egg products

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Embodiment 1

[0030] 1. Take a representative egg sample, boil it, mix thoroughly, weigh 2.0g into a 50mL centrifuge tube, add 5μL 13 C 6 - PCP internal standard solution (1.0mg / L), then add 8% (V / V) triethylamine in acetonitrile aqueous solution (70 / 30, V / V) extract 10mL, homogenize for 1min, ultrasonically extract for 10min, vortex Spin for 10 minutes, then centrifuge at 8500r / min for 5 minutes, draw 5mL of supernatant into a stoppered test tube, add 2mL of water, mix well, and wait for purification.

[0031] 2. Add the above extract to the mixed anion exchange column (6mL / 150mg) that has been activated and balanced with 5mL methanol and 5mL water, the magnetic aminated anion exchange composite material and common C18 filler are in a weight ratio of 80mg / 20mg), Control the flow rate to 2mL / min, then wash with 6mL methanol, 6mL water and 6mL formic acid / methanol / water solution (2 / 49 / 49, V / V / V) respectively, dry it with 10% (V / V ) methanol solution of formic acid in 10mL, collect the elua...

Embodiment 2

[0037] 1. Take a representative duck egg sample, cook it, mix it well, weigh 2.0g into a 50mL centrifuge tube, add 5μL of 13 C 6 - PCP internal standard solution (1.0mg / L), then add 8% (V / V) triethylamine in acetonitrile aqueous solution (70 / 30, V / V) extract 10mL, homogenize for 1min, ultrasonically extract for 10min, vortex Spin for 10 minutes, then centrifuge at 8500r / min for 5 minutes, draw 5mL of supernatant into a stoppered test tube, add 2mL of water, mix well, and wait for purification.

[0038] 2. Add the above extract to a mixed anion exchange column (6mL / 150mg, magnetic aminated anion exchange composite material and common C18 filler by weight ratio 80mg / 20mg) that has been activated and balanced with 5mL methanol and 5mL water, and control The flow rate is 2mL / min, then rinse with 6mL of methanol, 6mL of water and 6mL of formic acid / methanol / water solution (2 / 49 / 49, V / V / V), and dry it with 10% (V / V) The methanol solution of formic acid was eluted in 10 mL portions...

Embodiment 3

[0040] 1. Take a representative quail egg sample, cook it, mix it well, weigh 2.0g into a 50mL centrifuge tube, add 5μL 13 C 6 - PCP internal standard solution (1.0mg / L), then add 8% (V / V) triethylamine in acetonitrile aqueous solution (70 / 30, V / V) extract 10mL, homogenize for 1min, ultrasonically extract for 10min, vortex Spin for 10 minutes, then centrifuge at 8500r / min for 5 minutes, draw 5mL of supernatant into a stoppered test tube, add 2mL of water, mix well, and wait for purification.

[0041] 2. Add the above extract to a mixed anion exchange column (6mL / 150mg, magnetic aminated anion exchange composite material and common C18 filler by weight ratio 80mg / 20mg) that has been activated and balanced with 5mL methanol and 5mL water, and control The flow rate is 2mL / min, then rinse with 6mL of methanol, 6mL of water and 6mL of formic acid / methanol / water solution (2 / 49 / 49, V / V / V), and dry it with 10% (V / V) The methanol solution of formic acid was eluted in 10 mL portions, ...

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Abstract

A method for determination of the residual quantity of pentachlorophenol in eggs and egg products is characterized by comprising the steps: taking 1.0-5.0 g of a homogeneous sample in a 10 mL polypropylene centrifugal tube, adding 5-15 mL of an acetonitrile-water solution containing 5.0%-10.0% (V/V) of triethylamine, carrying out ultrasonic extraction and centrifugal separation, purifying the supernatant via a small mixed anion exchange column (6 mL), leaching with a methanol/water solution (50/50, V/V) containing 1.0%-5.0% (V/V) of formic acid, carrying out graded elution with a methanol solution containing 6.0%-15.0% (V/V) of formic acid, blowing the elution solution with nitrogen with the temperature of 40 DEG C to nearly dry, and redissolving with methanol for liquid chromatography tandem mass spectrometric determination. The method has the advantages of simple process, convenient and fast operation, good enrichment efficiency, high extraction recovery rate, low price, and good detection sensitivity and precision, is suitable for analysis of the residual quantity of pentachlorophenol in the eggs and the egg products, and has great significance on control of the residual quantity of pentachlorophenol in the eggs and the egg products and ensuring of food safety and human health.

Description

technical field [0001] The invention belongs to the technical field of food safety detection, and relates to a method for determining the residual amount of pentachlorophenol in poultry eggs and poultry egg products, more specifically, it relates to the extraction, Small column enrichment purification and liquid chromatography-tandem mass spectrometry determination. Background technique [0002] Pentachlorophenol (PCP) is a mutagen widely used as insecticide, herbicide, antibacterial agent and wood preservative, and its existence in the environment and food has attracted great attention of food safety experts. Poultry eggs are one of the main protein food sources for humans. Due to the pollution of the environment and feed during the feeding process, poultry eggs are often detected to contain pentachlorophenol residues. [0003] At present, although there are documents such as "Determination of Pentachlorophenol Residues in Animal Source Foods in National Food Safety Standa...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06G01N30/08
Inventor 金米聪陈晓红潘胜东赵永纲
Owner NINGBO MUNICIPAL CENT FOR DISEASE CONTROL & PREVENTION
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