Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Immunoaffinity chromatography-ultrahigh performance liquid chromatography-mass spectrum combined rapid detection method for perfluorinated compounds in dairy products

An ultra-high performance liquid phase and perfluorinated compound technology, which is applied in the field of detection of perfluorinated compounds in dairy products and water, can solve the problems of large difference in polarity, low recovery rate and high cost of use of PFCs

Inactive Publication Date: 2014-01-01
SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
View PDF0 Cites 16 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the extraction effect of these SPE columns is better than that of LLE, there are still some disadvantages: SPE columns are relatively expensive, although they can be reused in theory, but due to the complexity of environmental samples, they are often seldom reused, and the cost of use is relatively high; commercialization The packing of the SPE column is easily blocked by complex sample contamination, and the column efficiency is reduced; PFCs have large polarity differences, and reversed-phase or ion-exchange SPE packings are not suitable for all PFCs extraction, such as reversed-phase adsorbents are not sufficient for small molecular polar compounds Retention, composite weak ion-exchange sorbents, although taking into account both ion-exchange and reversed-phase mechanisms, are better than reversed-phase sorbents, but the recovery rate of perfluoroacid above C10 in tissues is less than 50%
After a new search, there is no research report on the immunoassay method and sample pretreatment IAC for PFCs

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Immunoaffinity chromatography-ultrahigh performance liquid chromatography-mass spectrum combined rapid detection method for perfluorinated compounds in dairy products
  • Immunoaffinity chromatography-ultrahigh performance liquid chromatography-mass spectrum combined rapid detection method for perfluorinated compounds in dairy products
  • Immunoaffinity chromatography-ultrahigh performance liquid chromatography-mass spectrum combined rapid detection method for perfluorinated compounds in dairy products

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1P

[0047] The preparation of embodiment 1PFOS immunoaffinity column

[0048] 1. Antibody Preparation

[0049] With reaction buffer (0.1mol / L, NaHCO 3 , 0.5mol / LNaCI, pH8.3) to dilute the antibody solution. Prepare 10 mL of 2 mg / mL antibody solution.

[0050] 2. Preparation of affinity column

[0051] Refer to the product manual of SepharoseCL 4B glue activated by cyanogen bromide (CNBr), the specific operation steps are as follows:

[0052] (1) Suspend 2g of CNBr-activated SepharoseCL4B dry gel in 20mL 1moL / L HCL for swelling, and then wash the swollen gel with about 200mL 1mmol / L HCL.

[0053] (2) Use 200mL of reaction buffer (0.1mol / L NaHCO 3 , pH 8.1) to wash thoroughly, add the gel to 10mL 2mg / mL PFOS antibody reaction buffer solution, stir gently at room temperature for 2h, let it stand, collect the reaction supernatant, and measure the uncoupled protein content in the eluate with a UV spectrophotometer , it was determined that the coupling rate of the prepared PFOS an...

Embodiment 2

[0056] Example 2 Using PFOS Immunoaffinity Chromatographic Columns to Process Milk Samples and LC-MS Detection and Analysis

[0057] The usage conditions of the affinity column prepared by the present invention are as follows: the sample loading volume is 50 mL, the sample loading flow rate is 2-3 mL / min, and 4 mL of acetonitrile is used as the elution solvent. For the milk samples where PFOS was not detected, three levels of PFOS were added at 0.01, 0.4 and 2.0ug / kg, respectively, and five average tests were performed at each level to detect the recovery rate and precision.

[0058] Use the following sample processing methods:

[0059] For milk samples where PFOS was not detected, add PFOS at three levels of 0.01, 0.4 and 2.0ug / L respectively, place the milk at 36°C to warm up, centrifuge at 7000r / min for 15min, discard the upper layer of milk fat and the lower layer of sediment, and transfer Take 50mL of the middle layer for sample loading (equivalent to 0.5ng, 20ng, 100ng ...

Embodiment 3

[0062] Example 3 Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry Determination of Standard Substances of Perfluorinated Compounds

[0063] Accurately draw 1mL of standard solution into a 100mL volumetric flask, dilute to volume with 7:3 methanol water, and shake well to obtain a 0.1mg / L standard working solution. Dilute step by step with 7:3 methanol water to obtain standard working solutions of 0.05mg / L, 0.005mg / L, 0.001mg / L, 0.0005mg / L, 0.0002mg / L, 0.00005mg / L, according to the mass concentration from dilute to Concentrated sequence is detected sequentially.

[0064] Use the ultra high performance liquid chromatography condition provided by the present invention to be:

[0065] Column: ACQUITY UPLC BEH C 18 2.1*50mm, or equivalent column.

[0066] Mobile phase: ①A: 5mmol / L ammonium acetate 5% methanol aqueous solution; ②Mobile phase B: 100% methanol. The gradient elution procedure is as follows:

[0067]

[0068] Column temperature: 45°C.

[0...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
recovery rateaaaaaaaaaa
Login to View More

Abstract

The invention relates to an immunoaffinity chromatography-ultrahigh performance chromatography-mass spectrum combined rapid detection method, and especially relates to a novel technology of a detection method for perfluorinated compounds in dairy products or water bodies. The method comprises following steps: step one, synthesis of artificial antigens; step two, screening and identification of polyclonal antibodies; step three, development of an immunoaffinity column; step four, establishment and optimizing of serially-combined detection method of ultrahigh performance liquid chromatography and mass spectrum. The technology provides a rapid detection method for perfluorinated compound residuals in the environment, improves the detection sensitivity, and guarantees the detection accuracy. The method meets the requirements on detection of perfluorinated compound residuals, and is beneficial for carrying out detections of perfluorinated compounds in real samples in the environment.

Description

technical field [0001] The invention relates to a rapid detection method combined with immunoaffinity chromatography-ultra-high performance liquid chromatography-mass spectrometry, in particular to a new technology for the detection method of perfluorinated compounds in dairy products and water bodies. Background technique [0002] Perfluorinated compounds (PFCs) are widely used in many industrial production and daily necessities such as polymer additives and lubricants due to their excellent thermal stability, chemical stability, high surface activity and hydrophobic and oleophobic properties. Perfluorooctane sulfonic acid (Perfluorooctane Sulphonate, PFOS) and perfluorooctanoic acid (Perfluorooctanoic Acid, PFOA) are representative PFCs. [0003] In May 2009, the United Nations Environment Program and the Fourth Conference of the Parties to the Stockholm Convention on Persistent Organic Pollutants (POPs) reached a consensus on reducing and finally banning the use of nine t...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/08G01N33/531
Inventor 朱江郭小品卢聪罗启仕杨洁孟梁朱杰郭琳李忠元张长波李青青王旌高洁朱悦
Owner SHANGHAI ACADEMY OF ENVIRONMENTAL SCIENCES
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com