This document describes methods for determining pesticide residues in foods. It discusses extracting pesticides from grains, fruits, vegetables, and milk using solvents like acetone and dichloromethane. The extracts are then cleaned up using chromatographic columns packed with materials like celite, carbon, and florisil. The cleaned extracts are analyzed using gas chromatography with detectors like FPD. The document provides operating conditions for GC and equations for calculating pesticide residue levels in foods based on peak heights. It also references several sources for additional information on pesticide residue analysis techniques.
In this slide contains pesticide used in grains, limits as per FSSAI , general detection method for pesticide in Grains and extraction procedures.
Presented by: P.Pavan Kalyan. (Department of pharmaceutical analysis).
RIPER, anantapur.
In this slides contains deep introduction about pesticides and analysis of pesticide residue in vegetables.
Presented by: M. Malarvannan (Department of pharmaceutical analysis),
RIPER, anantapur.
In this slide contains pesticide used in grains, limits as per FSSAI , general detection method for pesticide in Grains and extraction procedures.
Presented by: P.Pavan Kalyan. (Department of pharmaceutical analysis).
RIPER, anantapur.
In this slides contains deep introduction about pesticides and analysis of pesticide residue in vegetables.
Presented by: M. Malarvannan (Department of pharmaceutical analysis),
RIPER, anantapur.
Effects of pest and insects on various food, use of
pesticides in agriculture, pesticide cycle, organophosphorus and
organochlorine pesticides analysis, determination of pesticide residues in grain, fruits, vegetables, milk and milk products.
In this slides contains classification, mechanism of action, Pesticide Used in Agriculture and Quantification of Organophosphorus Pesticide.(food analysis).
Presented by: P. Naresh (Department of pharmaceutical analysis),
RIPER, anantapur.
As we all know chromatographic fingerprinting of botanicals is a quite recent concept. This presentation will help to the beginners to understand basic thories and fundamantals of thin layer chomatography. The presentation will also provide basic experiemental understanding to perfrom HPTLC fingerprinting of samples/extracts/formulations.
Regulatory requirement for setting herbal drug industryRAGHAV DOGRA
The World Health Organization (WHO) estimates that 80 percent of the population of some Asian and African countries presently use herbal medicine for some aspect of primary health care.Pharmaceuticals are prohibitively expensive for most of the world's population, half of whom lived on less than $2 U.S. per day in 2002. In comparison, herbal medicines can be grown from seed or gathered from nature for little or no cost
patent (/ˈpætənt/ or /ˈpeɪtənt/) is a set of exclusive rights granted by a sovereign state to an inventor or assignee for a limited period of time in exchange for detailed public disclosure of an invention. An invention is a solution to a specific technological problem and is a product or a process. Patents are a form of intellectual property.
MICROBIAL CONTAMINATION IN HERBS AND THEIR FORMULATIONSVK VIKRAM VARMA
INTRODUCTION
SOURCES OF CONTAMINATION
RAW MATERIALS
PACKAGING MATERIALS
LIMITS FOR MICROBIAL CONTAMINATION
LIMITS AS PER WHO
TYPES OF CONTAMINATION
DIRECT CONTAMINATION
CROSS CONTAMINATION
DETERMINATION OF CONTAMINATION
TOTAL VIABLE COUNT
PRETREATMENT OF HERBAL MATERIALS
REFRENCES
Join the experts as they discuss the use of accelerated solvent extraction and QuEChERS techniques for the extraction of pesticide residues from a diverse range of food samples. Tips and tricks for improving the extraction efficiency will be covered, along with selection criteria for each technique by sample type, assisting analysts in modifying existing methods or developing new methods to tackle their analytical challenges
In this slide contains need of food regulations, system and Legislation Regulation of Food Products as per BSI and Agmark.
Presented by: G. Chiranjeevi (Department of pharmaceutical analysis),
RIPER, anantapur.
In this slide contains adulteration, milk standards, sample preparation, identification of adulterants and contamination of milk.
Presented by: G.Sateesh Chandra (Department of pharmaceutical analysis).RIPER, anantapur
Effects of pest and insects on various food, use of
pesticides in agriculture, pesticide cycle, organophosphorus and
organochlorine pesticides analysis, determination of pesticide residues in grain, fruits, vegetables, milk and milk products.
In this slides contains classification, mechanism of action, Pesticide Used in Agriculture and Quantification of Organophosphorus Pesticide.(food analysis).
Presented by: P. Naresh (Department of pharmaceutical analysis),
RIPER, anantapur.
As we all know chromatographic fingerprinting of botanicals is a quite recent concept. This presentation will help to the beginners to understand basic thories and fundamantals of thin layer chomatography. The presentation will also provide basic experiemental understanding to perfrom HPTLC fingerprinting of samples/extracts/formulations.
Regulatory requirement for setting herbal drug industryRAGHAV DOGRA
The World Health Organization (WHO) estimates that 80 percent of the population of some Asian and African countries presently use herbal medicine for some aspect of primary health care.Pharmaceuticals are prohibitively expensive for most of the world's population, half of whom lived on less than $2 U.S. per day in 2002. In comparison, herbal medicines can be grown from seed or gathered from nature for little or no cost
patent (/ˈpætənt/ or /ˈpeɪtənt/) is a set of exclusive rights granted by a sovereign state to an inventor or assignee for a limited period of time in exchange for detailed public disclosure of an invention. An invention is a solution to a specific technological problem and is a product or a process. Patents are a form of intellectual property.
MICROBIAL CONTAMINATION IN HERBS AND THEIR FORMULATIONSVK VIKRAM VARMA
INTRODUCTION
SOURCES OF CONTAMINATION
RAW MATERIALS
PACKAGING MATERIALS
LIMITS FOR MICROBIAL CONTAMINATION
LIMITS AS PER WHO
TYPES OF CONTAMINATION
DIRECT CONTAMINATION
CROSS CONTAMINATION
DETERMINATION OF CONTAMINATION
TOTAL VIABLE COUNT
PRETREATMENT OF HERBAL MATERIALS
REFRENCES
Join the experts as they discuss the use of accelerated solvent extraction and QuEChERS techniques for the extraction of pesticide residues from a diverse range of food samples. Tips and tricks for improving the extraction efficiency will be covered, along with selection criteria for each technique by sample type, assisting analysts in modifying existing methods or developing new methods to tackle their analytical challenges
In this slide contains need of food regulations, system and Legislation Regulation of Food Products as per BSI and Agmark.
Presented by: G. Chiranjeevi (Department of pharmaceutical analysis),
RIPER, anantapur.
In this slide contains adulteration, milk standards, sample preparation, identification of adulterants and contamination of milk.
Presented by: G.Sateesh Chandra (Department of pharmaceutical analysis).RIPER, anantapur
Sterility testing products (solids, liquids, ophthalmic and other sterile pro...Ms. Pooja Bhandare
PHARMACEUTICAL MICROBIOLOGY (BP303T)Unit-IIIPart-6 Sterility testing products (solids, liquids, ophthalmic and other sterile products) according to IP, BP, USP.
Introduction: Test for Sterility. Culture Media. Fluid Thioglycollate Medium (FTM).
Alternative Thioglycollate Medium (ATM).
Soybean Casein Digest Medium (SCDM).
Tests for Culture Media:
Sterility of Media.
Growth Promotion Test.
Test for Bacteriostatic and Fungistatic.
Sterility Test Methods. Methods A: Membrane Filtration.
Method B: Direct Inoculation Pyrogen Test Methods. Rabbit Test. LAL Test.
It is generally recognized that stained fecal films are the single most productive means of stool examination for intestinal protozoa. The permanent stained smear facilitates detection and identification of cysts and trophozoites and affords a permanent record of the protozoa encountered. Small protozoa, missed by wet mount examinations (of either unconcentrated or concentrated samples) are often seen on the stained smear. The Wheatley Trichrome technique for fecal specimens is a modification of Gomori's original staining procedure for tissue. It is a rapid, simple procedure, which produces uniformly well-stained smears of the intestinal protozoa, human cells, yeast, and artifact material.
Ozempic: Preoperative Management of Patients on GLP-1 Receptor Agonists Saeid Safari
Preoperative Management of Patients on GLP-1 Receptor Agonists like Ozempic and Semiglutide
ASA GUIDELINE
NYSORA Guideline
2 Case Reports of Gastric Ultrasound
ARTIFICIAL INTELLIGENCE IN HEALTHCARE.pdfAnujkumaranit
Artificial intelligence (AI) refers to the simulation of human intelligence processes by machines, especially computer systems. It encompasses tasks such as learning, reasoning, problem-solving, perception, and language understanding. AI technologies are revolutionizing various fields, from healthcare to finance, by enabling machines to perform tasks that typically require human intelligence.
Couples presenting to the infertility clinic- Do they really have infertility...Sujoy Dasgupta
Dr Sujoy Dasgupta presented the study on "Couples presenting to the infertility clinic- Do they really have infertility? – The unexplored stories of non-consummation" in the 13th Congress of the Asia Pacific Initiative on Reproduction (ASPIRE 2024) at Manila on 24 May, 2024.
Anti ulcer drugs and their Advance pharmacology ||
Anti-ulcer drugs are medications used to prevent and treat ulcers in the stomach and upper part of the small intestine (duodenal ulcers). These ulcers are often caused by an imbalance between stomach acid and the mucosal lining, which protects the stomach lining.
||Scope: Overview of various classes of anti-ulcer drugs, their mechanisms of action, indications, side effects, and clinical considerations.
Title: Sense of Smell
Presenter: Dr. Faiza, Assistant Professor of Physiology
Qualifications:
MBBS (Best Graduate, AIMC Lahore)
FCPS Physiology
ICMT, CHPE, DHPE (STMU)
MPH (GC University, Faisalabad)
MBA (Virtual University of Pakistan)
Learning Objectives:
Describe the primary categories of smells and the concept of odor blindness.
Explain the structure and location of the olfactory membrane and mucosa, including the types and roles of cells involved in olfaction.
Describe the pathway and mechanisms of olfactory signal transmission from the olfactory receptors to the brain.
Illustrate the biochemical cascade triggered by odorant binding to olfactory receptors, including the role of G-proteins and second messengers in generating an action potential.
Identify different types of olfactory disorders such as anosmia, hyposmia, hyperosmia, and dysosmia, including their potential causes.
Key Topics:
Olfactory Genes:
3% of the human genome accounts for olfactory genes.
400 genes for odorant receptors.
Olfactory Membrane:
Located in the superior part of the nasal cavity.
Medially: Folds downward along the superior septum.
Laterally: Folds over the superior turbinate and upper surface of the middle turbinate.
Total surface area: 5-10 square centimeters.
Olfactory Mucosa:
Olfactory Cells: Bipolar nerve cells derived from the CNS (100 million), with 4-25 olfactory cilia per cell.
Sustentacular Cells: Produce mucus and maintain ionic and molecular environment.
Basal Cells: Replace worn-out olfactory cells with an average lifespan of 1-2 months.
Bowman’s Gland: Secretes mucus.
Stimulation of Olfactory Cells:
Odorant dissolves in mucus and attaches to receptors on olfactory cilia.
Involves a cascade effect through G-proteins and second messengers, leading to depolarization and action potential generation in the olfactory nerve.
Quality of a Good Odorant:
Small (3-20 Carbon atoms), volatile, water-soluble, and lipid-soluble.
Facilitated by odorant-binding proteins in mucus.
Membrane Potential and Action Potential:
Resting membrane potential: -55mV.
Action potential frequency in the olfactory nerve increases with odorant strength.
Adaptation Towards the Sense of Smell:
Rapid adaptation within the first second, with further slow adaptation.
Psychological adaptation greater than receptor adaptation, involving feedback inhibition from the central nervous system.
Primary Sensations of Smell:
Camphoraceous, Musky, Floral, Pepperminty, Ethereal, Pungent, Putrid.
Odor Detection Threshold:
Examples: Hydrogen sulfide (0.0005 ppm), Methyl-mercaptan (0.002 ppm).
Some toxic substances are odorless at lethal concentrations.
Characteristics of Smell:
Odor blindness for single substances due to lack of appropriate receptor protein.
Behavioral and emotional influences of smell.
Transmission of Olfactory Signals:
From olfactory cells to glomeruli in the olfactory bulb, involving lateral inhibition.
Primitive, less old, and new olfactory systems with different path
Lung Cancer: Artificial Intelligence, Synergetics, Complex System Analysis, S...Oleg Kshivets
RESULTS: Overall life span (LS) was 2252.1±1742.5 days and cumulative 5-year survival (5YS) reached 73.2%, 10 years – 64.8%, 20 years – 42.5%. 513 LCP lived more than 5 years (LS=3124.6±1525.6 days), 148 LCP – more than 10 years (LS=5054.4±1504.1 days).199 LCP died because of LC (LS=562.7±374.5 days). 5YS of LCP after bi/lobectomies was significantly superior in comparison with LCP after pneumonectomies (78.1% vs.63.7%, P=0.00001 by log-rank test). AT significantly improved 5YS (66.3% vs. 34.8%) (P=0.00000 by log-rank test) only for LCP with N1-2. Cox modeling displayed that 5YS of LCP significantly depended on: phase transition (PT) early-invasive LC in terms of synergetics, PT N0—N12, cell ratio factors (ratio between cancer cells- CC and blood cells subpopulations), G1-3, histology, glucose, AT, blood cell circuit, prothrombin index, heparin tolerance, recalcification time (P=0.000-0.038). Neural networks, genetic algorithm selection and bootstrap simulation revealed relationships between 5YS and PT early-invasive LC (rank=1), PT N0—N12 (rank=2), thrombocytes/CC (3), erythrocytes/CC (4), eosinophils/CC (5), healthy cells/CC (6), lymphocytes/CC (7), segmented neutrophils/CC (8), stick neutrophils/CC (9), monocytes/CC (10); leucocytes/CC (11). Correct prediction of 5YS was 100% by neural networks computing (area under ROC curve=1.0; error=0.0).
CONCLUSIONS: 5YS of LCP after radical procedures significantly depended on: 1) PT early-invasive cancer; 2) PT N0--N12; 3) cell ratio factors; 4) blood cell circuit; 5) biochemical factors; 6) hemostasis system; 7) AT; 8) LC characteristics; 9) LC cell dynamics; 10) surgery type: lobectomy/pneumonectomy; 11) anthropometric data. Optimal diagnosis and treatment strategies for LC are: 1) screening and early detection of LC; 2) availability of experienced thoracic surgeons because of complexity of radical procedures; 3) aggressive en block surgery and adequate lymph node dissection for completeness; 4) precise prediction; 5) adjuvant chemoimmunoradiotherapy for LCP with unfavorable prognosis.
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Pulmonary Thromboembolism - etilogy, types, medical- Surgical and nursing man...VarunMahajani
Disruption of blood supply to lung alveoli due to blockage of one or more pulmonary blood vessels is called as Pulmonary thromboembolism. In this presentation we will discuss its causes, types and its management in depth.
- Video recording of this lecture in English language: https://youtu.be/lK81BzxMqdo
- Video recording of this lecture in Arabic language: https://youtu.be/Ve4P0COk9OI
- Link to download the book free: https://nephrotube.blogspot.com/p/nephrotube-nephrology-books.html
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Report Back from SGO 2024: What’s the Latest in Cervical Cancer?bkling
Are you curious about what’s new in cervical cancer research or unsure what the findings mean? Join Dr. Emily Ko, a gynecologic oncologist at Penn Medicine, to learn about the latest updates from the Society of Gynecologic Oncology (SGO) 2024 Annual Meeting on Women’s Cancer. Dr. Ko will discuss what the research presented at the conference means for you and answer your questions about the new developments.
The prostate is an exocrine gland of the male mammalian reproductive system
It is a walnut-sized gland that forms part of the male reproductive system and is located in front of the rectum and just below the urinary bladder
Function is to store and secrete a clear, slightly alkaline fluid that constitutes 10-30% of the volume of the seminal fluid that along with the spermatozoa, constitutes semen
A healthy human prostate measures (4cm-vertical, by 3cm-horizontal, 2cm ant-post ).
It surrounds the urethra just below the urinary bladder. It has anterior, median, posterior and two lateral lobes
It’s work is regulated by androgens which are responsible for male sex characteristics
Generalised disease of the prostate due to hormonal derangement which leads to non malignant enlargement of the gland (increase in the number of epithelial cells and stromal tissue)to cause compression of the urethra leading to symptoms (LUTS
2. DETERMINATION OF PESTICIDE RESIDUES
IN
• GRAINS
• FRUITS
• VEGETABLES
• MILK & ITS PRODUCTS
CONT. WITH PESTICIDE ANALYSIS
3. WHAT ISPESTICIDE RESIDUES?
When a crop istreated with a pesticide, a very small amountof the
pesticide, or its metabolites or degradation products, can remain in
thecrop until after it is harvested.
4. WHY DO THEY TURN UP IN OUR
FOOD?
• To control the growth of weeds usedby farmers or
prevent crop damage by insects,rodents and molds.
• usedonfood crops after harvest to prolong their
storagelife.
• usedonanimal farms to control insect pests
6. DOPROCESSEDFOODSHAVELESS PESTICIDES
THANFRESHFOODS?
Generally, yes.
Reason:
Growers : don’t need to ensure that their foods are
cosmetically perfect
Processors: consumerdemand for foods with minimal
pesticide residues
Processing : reduce pesticide residues
10. EFFECTOF CHEMICAL SOLUTIONS ON PESTICIDE
RESIDUES
Acidic solutions
ascorbic acid
acetic acid
hydrogen peroxide
citric acid
At a concentration of 5 and 10 percent for 10 minutes reduction of pesticide residues.
11. ALKALINE SOLUTION
Dipping of fruits in NaOH solutionremoves 50 to 60 percent surface residuesof pyrethroids
compared to 40 to 50 percent removed by hydrolytic degradation with NaOH and a detergent
solutionremoved 50 to 60 percent residues,along with thissoap are usedas decontaminating agents
Solutions of NaOH, acetic acid, potassium dichromate
12. OZONATION
Ozone because of its powerful oxidizing property iseffectively applied in
drinking water and waste water treatment
Tapwater treatment + ozonated water treatments significantly reduced
the pesticide residues onvegetables, ascompared to no-wash treatment
pesticide residues
13. NEUTRAL SOLUTIONS
Sodiumchloride (NaCl)solution
28 to 93% organochlorines
100 % organophoshates
NaCl concentration pesticide residues
5 and 10 % NaCl solution
for 15 minutes rubbed by
hand & water was decanted
14. WHAT CANYOUDO?
Grow someof your food usingorganicmethods.
Buyorganicfood.
Washand scruball fresh fruits, vegetables
Eatlessor no meat.
Trimthe fat frommeat.
16. Apparatus
A.
A gas chromatograph equipped with flame
photometric detector operated in phosphorus
mode (FPD-P), 526 mm filter.
i. Operating conditions:
Injector temperature 220°C
Baseline noise should be < 2%
ii. Columns :
SPB-5 (Supelco, Bellefonte, PA) or
any equivalent 30m x 0.53mm
N2 carrier gas
17. B. Chromatographic cleanup columns:
Ready to use Extrelut-3, needle is fixed at column end as flow regulator.
Glass column 30cm x 20 mm with glass septum (Carbon-celite cleanup).
C. Chopper grinder.
19. Reagents
i. Reference standard solutions: prepared using heptane or n-hexane (benzene is
added if solubilization is difficult)
ii. Solvents: Acetone, acetonitrile, benzene, dichloromethane, methanol, n-hexane
(All HPLC grade).
iii. Silanized glass wool.
iv. Celite 545.
v. Active carbon.
vi. Sodium Chloride.
vii.Cotton wool washed with acetone and n-hexane.
20. Pesticide standard solutions:
i. Stock solutions of 1mg/ml using ethyl acetate.
ii. Working solution of 0.5μg/ml.
Extraction:
Foods are divided into three main groups according to moisture and fat content-
i. Group I (Vegetables and fruits):
50g of chopped sample is added into high speed blender jar.
100ml of acetone
Blended for 2 mins at high speed.
Filtered with Buchner funnel.
Washed with 50ml acetone.
Extract brought to 150-200ml volume with acetone : water (2:1).
21. ii. Group II (Milk):
100ml milk is taken in a separatory funnel.
150ml acetone is added.
Extracted first with 100ml methylene chloride.
Then again with 50ml of same.
Extract is dried over anhydrous sodium sulfate
at 50-60°C, under reduced pressure.
iii. Group III (Grains):
50gm chopped sample into high speed blender jar.
50 ml distilled water added.
Filtered with Buchner funnel.
Washed with 50ml acetone.
Extract brought to 150-200ml volume with acetone :
water (2:1).
22. Partition
• For all groups ( 1 & 2 ) half the volume of food extract equivalent to 25g of sample is placed
in a separating funnel.
• 100ml of dichloromethane, 100ml of acetone and 10g of sodium chloride is added.
• Shaken vigorously till most sodium chloride is dissolved.
• Layers are allowed to separate.
To aqueous layer
• The Aqueous layer is transferred to a second separatory funnel.
• 200ml of dichloromethane is added to the second separatory funnel.
Organic layer
• Organic layer is dried through sodium sulfate.
• The organic layer is dried.
• All organic layers are collected and concentrated just to dryness in rotary vacuum evaporator.
23. Chromatographic column clean up
i. Group I and II
Glass column is filled with 2g celite.
4g of carbon:celite (1:4) is added.
Topped with glass wool plug.
Column is washed with 20ml benzene.
Sample is transferred quantitatively with small portions of benzene.
Pesticide is eluted with 60ml of acetonitrile-benzene (1:1).
Concentrated just to dryness in rotary vacuum evaporator.
Suitable amount of benzene is added and analyzed by GC.
ii. Group II
Sample is transferred quantitatively to disposable Extrelut-3 with 3ml of n-hexane.
Solution is allowed to drain into filling material.
Waited for 10mins to obtained even distribution.
Eluted three times with 5ml acetonitrile-n-hexane (1:1).
Concentrated just to dryness in rotary vacuum evaporator.
Suitable amount of benzene is added and analyzed by GC.
24. Determination
Residues are quantified by height or area measurement from solution of known
concentration of authentic compounds.
Compounds Column
SPB-5 SP2250-SP2401
Acephate 0.26 0.97
Chlorpyriphos 1.18 0.82
Ethion 1.73 1.09
Monocrotophos 0.64 0.9
Paraoxon 1.06 1.08
Parathion 1.19 19
Pirimiphos-methyl 1.11 0.97
Table. GC retention times (min) for some organophosphorus insecticides relative to parathion-
methyl.
25. Calculation
Residue level
mg
kg
=
h1 v1 V
h2 v2 m
𝑐
Where,
h1= peak height of the sample
h2= peak height of the standard
v1= μl of the standard injected
v2= μl of the extract injected
V= final volume of the sample extract (ml)
m= mass in g of the sample
c= concentration in ppm of reference solution.
27. Apparatus
i. Refrigerated centrifuge; able to rotate at
3000rpm at 15°C.
ii. SPE (Solid phase extraction)
automatic
iii. Rotary vacuum evaporator.
iii. Gas chromatograph system with
injection device and electron capture
detector.
28. v. Capillary column- nonpolar dimethyl polysiloxane, thickness 0.25μg, 50m x
0.32mm.
vi. Pre-column - 1.5m x 0.32mm.
vii.Volumetric pipettes.
29. Reagents
• Pesticide standard solution in hexane
• Acetone
• Diethyl ether Petroleum ether
• n-hexane
• Acetonitrile
• Methanol
• Methyl chloride
• Dodecane
• Sodium sulfate anhydrous
• Filter paper
• Nonpolar SPE cartridge
• Polar SPE cartridge
• Mobile phase- Helium 99.99% purity;
filtered for oxygen and water
30. General fat extraction
i. For milk:
50ml milk + 5ml methanol + 0.5g sodium oxalate, in separating funnel and shaken.
20ml diethyl ether is added and shaken again.
Repeated with 25ml petroleum ether.
Centrifuged for 5 mins at 1500rpm for 5 mins.
Organic phase is transferred into another separating funnel.
Aqueous phase is extracted twice with 50ml portions of ether and petroleum ether (1:1).
Combined solvent extracts washed over sodium sulfate anhydrous layer.
Evaporated using rotary vacuum evaporator at 35°C.
31. ii. For fish:
50ml of n-hexane + 20g of sample.
Mixed and centrifuged for 5 mins at 1500rpm.
Upper phase is decanted.
Extraction is repeated with another 50ml of n-hexane.
The two extracts are kept together.
Solvent evaporated at 35°C to 1ml.
Evaporation is finished with a gentle stream of nitrogen.
`
32. iii. For eggs:
A beaker is taken.
15g sand + 15g sodium sulfate anhydrous + 10g sample is taken in the beaker and
mixed.
A glass column with cotton wool swab is taken.
Sodium sulfate anhydrous is poured till 2cm of the column.
The contents of the beaker are poured in.
Eluted with 170ml n-hexane and acetone (2:1).
Solvent evaporated at 35°C to 1ml.
Evaporation is finished with a gentle stream of nitrogen.
33. Gas chromatographic determination
Operation conditions:
Helium as mobile phase at 23 psi.
Initial oven temperature at 100°C, holding time 2 min.
Initial injector temperature at 50°C.
Detector temperature at 320°C.
Injection volume 1μl.
Calculation Residue level
mg
kg
=
h1 v1 V
h2 v2 m
𝑐
Where,
h1= peak height of the sample
h2= peak height of the standard
v1= μl of the standard injected
v2= μl of the extract injected
V= final volume of the sample extract (ml)
m= mass in g of the sample
c= concentration in ppm of reference solution.
34. REFERENCES:
www.google.com
Slideshares.in
Tadeo, J. L. Analysis of Pesticides in Food and Environmental Samples. CRC Press, New York. 2008. 3:10:19:20.
Ministry of Health and Family Welfare, Government of India. fssai Manual of Methods of Analysis of Foods
Pesticide Residues. 2012, Lab manual 11. 70-77:116-120.
Matolcsy, G, Nadasy, M and Andriska, V. Pesticide Chemistry. Elsevier Science Publishing Co. Inc., New York.
1988 (32). 108:15-16.
35.
36. Clean up
i. C18 SPE:
Cartridge is processed twice with 5ml petroleum + 5ml acetone + 5ml methanol.
Eluted to meniscus.
Solution A is loaded into the cartridge.
Eluted to meniscus (kept for 3 mins in contact).
Container of Solution A is washed with 10ml acetonitrile and loaded into the cartridge and
eluted.
Elutant is evaporated at about 35°C with dodecane.
Diluted in n-hexane. (Solution B)
ii. Florisil SPE:
Cartridge is processed with 10ml n-hexane and eluted to meniscus.
Solution B is loaded.
Eluted with 10ml petroleum ether-diethyl ether (98:2) and 12ml of petroleum ether-diethyl
ether (85:15).
The two fractions are mixed together.
Evaporated together with 100μl dodecane.
Final extract dissolved in appropriate volume of n-hexane for GC analysis. (Solution C)
Editor's Notes
Friuts, vegetables, milk 1 and 2
IMP : u have to clea up the chromatographic column as similarly u did for the organophosphoroous pesticides