Introduction to qu e chers

Apr 4, 2013Download as PPTX, PDF6 likes3,830 views

This document provides an overview of the QuEChERS method for extracting pesticide residues from high water content food matrices: [1] QuEChERS stands for "Quick, Easy, Cheap, Effective, Rugged, and Safe" and was originally developed in 2001 for veterinary drug residue analysis. It has since been validated as a multiresidue method for pesticide residue analysis in plant materials. [2] The method uses acetonitrile extraction followed by dispersive solid phase extraction (DSPE) for cleanup. DSPE removes water and unwanted contaminants using bulk salts and sorbent mixtures like primary secondary amine (PSA) and magnesium sulfate. [

Introduction
to QuEChERS

Pradeep Kumar. G.T

QuEChERS (“catchers”)
Quick
Easy
Cheap
Effective
Rugged
Safe

 The QuEChERS-method was
developed by Michelangelo in the
year 2001 for the analysis of
veterinary drugs in animal tissues.

After realizing its great potential in the extraction of
polar and particularly basic compounds it was also
tested on pesticide residue analysis in plant material
with great success.



 Now QuEChERS is known as a
multiclass, multiresidue method (MRM)
for analysis of pesticides from high
water content (80-95%) matrices.

 The QuEChERS method now published
as AOAC method 2007.01
“Determination of Pesticide Residues in
Foods by Acetonitrile Extraction and
Partitioning with Magnesium Sulfate”.

T�� preferred solvent is
acetonitrile because it has been
shown to provide extraction of
the broadest range of organic
compounds without co-extraction
of large amounts of lipophilic
material.
This method is validated for the
analysis pesticide residue in dry
products like cereals, dried fruits,
tea and fatty foods like fish, meat.

Step 1: Sample preparation
and extraction
 Commodities are uniformly
ground
 Extract using required quantity of
acetonitrile
 Centrifuge the extract

 Cleaned up using DSPE.
 Bulk drying salts and DSPE sorbent
packings.
Remove excess water and unwanted
contaminants.
 Agitation and centrifugation
Vortex mixing for 30sec and
centrifuge at 3000 rpm for 5min

 Freezing out
The acetonitrile phase is
transferred into a centrifuge tube and
stored in a freezer (min 2hrs)
removal of lipids, waxes, sugars, and
other matrix co-extractives with low
solubility in acetonitrile.
follow DSPE.

 D-SPEwith a PSA/MgSO4-
mixture (for most samples)
The acetonitrile phase is
transferred into a PP-
centrifugation tube already
containing PSA and
magnesium sulfate and
agitate.

SPE DSPE
(Solid Phase Extraction) (Dispersive Solid Phase
Extraction)

Required 30 minutes to 1hr Few minutes
to complete

 This type of cleanup is recommended
for extracts of test samples containing
more than 50 mg of lipids.

 removal of chlorophyll and carotenoids .
 Samples like red sweet pepper, spinach and
vine leaves.

 Concentration of the extract in
Turbovap evaporator (2 to 5 mL)
 made up to volume with suitable
solvent.
 For GC n-Hexane is used and for
LC methanol.
 Analysis was done either by
GC/MS or LC/MS

Advantage
Conventional method QuEChERS
Time-Consuming, Complicated Simplified Alternatives
or Error-prone Steps
Sample No Way Around this
Processing/Homogenization
Blending/shaking for long time Homogenisation for 30 Sec
Filtration Centrifugation
Multiple Partitioning Steps Single Partitioning (“On-line”-
Approach)
Separation/Transfers of Entire Take Aliquots
Extract
Use of a Lot of Glassware A few glassware
Evaporation/Reconstitution of Evaporation/Reconstitution of
large volume small volume
Classical Steps/Classical SPE with Dispersive SPE
Columns & Manifold

Procedure schematically
(for 25 g sample)

Weigh 25 g sample into a 250 ml centrifuge
bottle (with screw cap)

Add 50 ml acetonitrile and shake well

Homogenise for 30 Sec (1st .
extraction step)

Add 10 g NaCl, shake each tube to dissolve
salt.

5g Na2SO4 added to an aliquot

From above step an aliquot is transferred to
mixture of 0.2g PSA and 0.75g MgSO4

Mix well in vortex (2nd extraction with
phase separation)

Centrifuge for 5 min at 3000 U/min

Aliquot is concentrated and reconstituted.

References

www.quechers.com

http://www.eurl-pesticides-datapool.eu/

1. The document discusses QuEChERS sample preparation and cleanup methods using different sorbents to remove interferents like fatty acids, pigments, and sterols from pesticide extracts. 2. It evaluates the effectiveness of a new engineered carbon material called CarbonX compared to traditional glass-backed carbon sorbent for removing contaminants while maintaining high pesticide recoveries and minimizing column and liner fouling during GC/MS analysis. 3. The CarbonX material showed superior recoveries of planar pesticides above 75% and was able to remove extreme fatty acid contaminants from botanical extracts, demonstrating its potential to handle difficult sample matrices compared to other cleanup methods.

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This document describes procedures for extracting important phytochemicals from various plants. It includes extraction methods for isolating starch from potatoes, calcium citrate from lemons, piperine from black pepper, caffeine from tea, curcumin from turmeric, capsaicin from red chili powder, and standardization of the extracts using TLC. The conclusion states that phytochemical analysis confirmed the presence of the claimed secondary metabolites in the various plant extracts. Extraction yields ranging from 0.76% to 7.2% were obtained.

A Report On Instrumental analysis Done in PhilMechJanine Samelo

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The Philippine Center for Postharvest Development and Mechanization (PHilMech) conducts agricultural research and analysis to develop postharvest technologies. Its chemistry laboratory analyzes samples to ensure food safety and quality. Analyses include determining chlorophyll content using UV-Vis spectrophotometry and detecting aflatoxin B1, a carcinogenic mold toxin, using high-performance liquid chromatography. The laboratory has two trained chemists and uses instruments like a UV-Vis spectrophotometer and HPLC to precisely analyze samples according to standardized methods. Results are evaluated to ensure quality control.

Pressurized accelerated extraction of pollutantsBhupander Kumar

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Accelerated solvent extraction (ASE) is a technique that uses solvents, elevated temperatures, and pressures to efficiently extract analytes from solid samples. It provides several advantages over traditional techniques like Soxhlet extraction, including requiring smaller sample and solvent volumes and shorter extraction times. Key factors that influence ASE extraction include sample preparation, solvent selection, temperature, pressure, static time, flush volume, and number of cycles. These parameters require optimization for different sample matrixes and target analytes. ASE is useful for extracting pesticides, PAHs, PCBs, and dioxins from soils, sediments, plants and other solid environmental samples.

www.eco-web.com_edi_03336-02.htmlDr. Mukesh Raikwar

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1) A sensitive method for detecting chlormequat chloride (CCC) residues in foods like fruits, vegetables and grains using liquid chromatography-mass spectrometry (LC-MS) was developed. 2) The method involved homogenizing samples, extracting with methanol containing formic acid, and analyzing by LC-MS in multiple reaction monitoring mode. Recoveries from spiked samples ranged from 83-96% with good precision. 3) The method was validated according to parameters like linearity, limits of detection/quantification, repeatability and reproducibility. CCC residues detected in real samples from India were mostly below regulatory limits, except in some grapes and okra.

Improvement of solubility and oral bioavailability of curcuminthamrooks

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Curcumin has numerous biological activities but has poor solubility and low oral bioavailability. To address these issues, curcumin can be formulated into nanostructures like nanocapsules. This document describes a study where curcumin was encapsulated into chitosan nanocapsules using ionotropic gelation. Chitosan with a molecular weight of 710,000 Da produced nanocapsules around 197 nm in size that had high entrapment efficiency of curcumin. In vitro studies showed a fast release of curcumin. In vivo studies in mice found the oral bioavailability of curcumin from these nanocapsules was higher than curcumin alone, and they could cross the blood

54.Isolation and purification of cellulase from Aspergillus terreusAnnadurai B

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This document describes the isolation and purification of cellulase enzymes from the fungus Aspergillus terreus. The intracellular cellulase was purified using ammonium sulfate precipitation, DEAE-cellulose chromatography, and gel filtration chromatography. This purification scheme achieved a 270-fold purification with a 22.11% yield. Tests including PAGE, SDS-PAGE, immunodiffusion, and isoelectric focusing confirmed the homogeneity of the purified enzyme. The purified cellulase showed optimal activity between pH 4-7 and temperatures of 40-50°C.

Basics of PhytochemistryAshokrao Mane college of Pharmacy Peth-Vadgaon

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The document discusses various concepts and techniques used in phytochemistry including modern extraction methods like maceration, percolation, Soxhlet extraction and supercritical fluid extraction. It also covers isolation and purification techniques like fractional crystallization, distillation and sublimation. Methods of separation like paper chromatography, thin layer chromatography, gas chromatography and various spectroscopy techniques for identification are summarized.

ExtractionYassos Osman

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Sample preparation for Chromatography latha13061996

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1. The document discusses various sample preparation techniques for GC-MS and LC-MS analysis including headspace sampling, pyrolysis, solid phase extraction, automated solid phase extraction, solvent extraction, and accelerated solvent extraction. 2. For LC-MS analysis, common sample preparation techniques discussed are solid phase extraction, liquid-liquid extraction, protein precipitation extraction, desalting, isoelectric point precipitation, and organic solvent extraction. 3. Specific details are provided on steps involved in sample preparation for GC-MS analysis of THC as well as solid phase extraction, liquid-liquid extraction, and protein precipitation extraction techniques.

Analysis of organic acetates in e-vapor products by GC-MS/MSRana Tayyarah

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Analytical toxicologyPankaj Sonsurkar

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Final Paper ExperimentalNicholas Amado

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Pesticides 1romilaromila123

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Supercritical Fluid extraction Jasmine Kaur

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Automated Online Extraction and Chromatography with Supercritical FluidsShimadzu Scientific Instruments

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Characterization of β-Glucan from Oyster Mushroom (Pleurotus pulmonarius)BRNSSPublicationHubI

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Solid phase extraction & cold vapor atomic absorption spectrometryanitaelahi

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Proximate and non-proximate parameters analysis of food.pptxMasresha Minuye

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Rasp 1 93 rapid andsimplemethodmovvamounika

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extraction of important phytodrugMilantirtha Mete

��

A Report On Instrumental analysis Done in PhilMechJanine Samelo

��

Pressurized accelerated extraction of pollutantsBhupander Kumar

��

www.eco-web.com_edi_03336-02.htmlDr. Mukesh Raikwar

��

Improvement of solubility and oral bioavailability of curcuminthamrooks

��

54.Isolation and purification of cellulase from Aspergillus terreusAnnadurai B

��

Basics of PhytochemistryAshokrao Mane college of Pharmacy Peth-Vadgaon

��

ExtractionYassos Osman

��

Sample preparation for Chromatography latha13061996

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Analysis of organic acetates in e-vapor products by GC-MS/MSRana Tayyarah

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Introduction to qu e chers

1. Introduction to QuEChERS Pradeep Kumar. G.T

2. QuEChERS (“catchers”) Quick Easy Cheap Effective Rugged Safe

4.  The QuEChERS-method was developed by Michelangelo in the year 2001 for the analysis of veterinary drugs in animal tissues. After realizing its great potential in the extraction of polar and particularly basic compounds it was also tested on pesticide residue analysis in plant material with great success. 

5.  Now QuEChERS is known as a multiclass, multiresidue method (MRM) for analysis of pesticides from high water content (80-95%) matrices.  The QuEChERS method now published as AOAC method 2007.01 “Determination of Pesticide Residues in Foods by Acetonitrile Extraction and Partitioning with Magnesium Sulfate”.

6. T�� preferred solvent is acetonitrile because it has been shown to provide extraction of the broadest range of organic compounds without co-extraction of large amounts of lipophilic material. This method is validated for the analysis pesticide residue in dry products like cereals, dried fruits, tea and fatty foods like fish, meat.

7. Step 1: Sample preparation and extraction  Commodities are uniformly ground  Extract using required quantity of acetonitrile  Centrifuge the extract

8.  Cleaned up using DSPE.  Bulk drying salts and DSPE sorbent packings. Remove excess water and unwanted contaminants.  Agitation and centrifugation Vortex mixing for 30sec and centrifuge at 3000 rpm for 5min

9.  Freezing out The acetonitrile phase is transferred into a centrifuge tube and stored in a freezer (min 2hrs) removal of lipids, waxes, sugars, and other matrix co-extractives with low solubility in acetonitrile. follow DSPE.

10.  D-SPEwith a PSA/MgSO4- mixture (for most samples) The acetonitrile phase is transferred into a PP- centrifugation tube already containing PSA and magnesium sulfate and agitate.

11. SPE DSPE (Solid Phase Extraction) (Dispersive Solid Phase Extraction) Required 30 minutes to 1hr Few minutes to complete

12.  This type of cleanup is recommended for extracts of test samples containing more than 50 mg of lipids.

13.  removal of chlorophyll and carotenoids .  Samples like red sweet pepper, spinach and vine leaves.

14.  Concentration of the extract in Turbovap evaporator (2 to 5 mL)  made up to volume with suitable solvent.  For GC n-Hexane is used and for LC methanol.  Analysis was done either by GC/MS or LC/MS

15. Advantage Conventional method QuEChERS Time-Consuming, Complicated Simplified Alternatives or Error-prone Steps Sample No Way Around this Processing/Homogenization Blending/shaking for long time Homogenisation for 30 Sec Filtration Centrifugation Multiple Partitioning Steps Single Partitioning (“On-line”- Approach) Separation/Transfers of Entire Take Aliquots Extract Use of a Lot of Glassware A few glassware Evaporation/Reconstitution of Evaporation/Reconstitution of large volume small volume Classical Steps/Classical SPE with Dispersive SPE Columns & Manifold

16. Procedure schematically (for 25 g sample) Weigh 25 g sample into a 250 ml centrifuge bottle (with screw cap) Add 50 ml acetonitrile and shake well

17. Homogenise for 30 Sec (1st . extraction step) Add 10 g NaCl, shake each tube to dissolve salt. 5g Na2SO4 added to an aliquot From above step an aliquot is transferred to mixture of 0.2g PSA and 0.75g MgSO4

18. Mix well in vortex (2nd extraction with phase separation) Centrifuge for 5 min at 3000 U/min Aliquot is concentrated and reconstituted.

19. References www.quechers.com http://www.eurl-pesticides-datapool.eu/

21.  GCB-Graphitised Carbon Black

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Introduction to qu e chers

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