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.
irrational usage of pesticide leads to development of resistance, resurgence and toxic residue problems in our food. ultimately imbalance of environment . so that detection of pesticide residue in all materials of earth especially in our food, milk, meat, water, soil aquatic ecosystem and agriculture land. for the analysis of resiude set of procedure, methods, instruments, skills and laboratory must required. In this seminar would like to enlighten the best, suitable and feasible methods are discussed.
Pesticide residue analysis by simran.pptxSimran Bhatia
INTRODUCTION
The importance of food quality has become a serious issue due to the widespread use of pesticides. Though, the farmers have a conventional understanding of agriculture; they lack in the technical understanding of pesticides, their uses and safety aspects which makes them vulnerable (FAO, 2011).
Pesticide Residue: - The amount of insecticide left over after a lapse of time.” Disappearance of pesticide residue takes place by two ways i.e. Dissipation (In which the disappearance of the residue is fast) and Persistence (ability of pesticide to remain present for a long time).
Steps in Pesticide residue analysis:-
Sampling (collection, transport & storage)
Sample Preparation (Chopping/grinding/blending)
Extraction : Removal of pesticide residue from components that are present naturally
Clean-up : Removal of constituents that interfere with analysis of the pesticide residue of interest (Partitioning and purification )
Identification (detection), Quantification (determination) & Confirmation
4. EXTRACTION__________________________________________________________
Extraction is the process by which toxicant is transferred from the treated bulky biological material in to a solvent.
Principle : LIKE DISSOLVES LIKE and OPPOSITES DO NOT ATTRACT
QuEChERS_________________________________________________________________
Quick, Easy, Cheap, Effective, Rugged, and Safe.
◦ Developed in 2001 by American scientist Michelangelo
◦ Based on Acetonitrile extraction
◦ cleanup using dispersive-solid phase extraction (d-SPE) using MgSO4 and further purification with PSA and silica sorbent C18
◦ This method became popular because of its microscale extraction procedure which is simpler, consumes less time and organic solvent than all the previous methods.
Flow chart for QuEChERS sample preparation technique for pesticide residue analysis in FRUITS AND VEGETABLES
Status of Maximum Residue Limits in India:
The Central Insecticides Board and Registration Committee (CIBRC) registers pesticides in India and recommends them for various crops.
A total of 234 pesticides have been registered by CIBRC (including Endosulfan* the use of which was banned in India in May 2011).
Food Safety and Standard Authority of India (FSSAI) is responsible for setting MRLs for the pesticides that have been registered by CIBRC.
The MRLs for all registered pesticides should be set for all the crops they have been registered.
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.
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.
irrational usage of pesticide leads to development of resistance, resurgence and toxic residue problems in our food. ultimately imbalance of environment . so that detection of pesticide residue in all materials of earth especially in our food, milk, meat, water, soil aquatic ecosystem and agriculture land. for the analysis of resiude set of procedure, methods, instruments, skills and laboratory must required. In this seminar would like to enlighten the best, suitable and feasible methods are discussed.
Pesticide residue analysis by simran.pptxSimran Bhatia
INTRODUCTION
The importance of food quality has become a serious issue due to the widespread use of pesticides. Though, the farmers have a conventional understanding of agriculture; they lack in the technical understanding of pesticides, their uses and safety aspects which makes them vulnerable (FAO, 2011).
Pesticide Residue: - The amount of insecticide left over after a lapse of time.” Disappearance of pesticide residue takes place by two ways i.e. Dissipation (In which the disappearance of the residue is fast) and Persistence (ability of pesticide to remain present for a long time).
Steps in Pesticide residue analysis:-
Sampling (collection, transport & storage)
Sample Preparation (Chopping/grinding/blending)
Extraction : Removal of pesticide residue from components that are present naturally
Clean-up : Removal of constituents that interfere with analysis of the pesticide residue of interest (Partitioning and purification )
Identification (detection), Quantification (determination) & Confirmation
4. EXTRACTION__________________________________________________________
Extraction is the process by which toxicant is transferred from the treated bulky biological material in to a solvent.
Principle : LIKE DISSOLVES LIKE and OPPOSITES DO NOT ATTRACT
QuEChERS_________________________________________________________________
Quick, Easy, Cheap, Effective, Rugged, and Safe.
◦ Developed in 2001 by American scientist Michelangelo
◦ Based on Acetonitrile extraction
◦ cleanup using dispersive-solid phase extraction (d-SPE) using MgSO4 and further purification with PSA and silica sorbent C18
◦ This method became popular because of its microscale extraction procedure which is simpler, consumes less time and organic solvent than all the previous methods.
Flow chart for QuEChERS sample preparation technique for pesticide residue analysis in FRUITS AND VEGETABLES
Status of Maximum Residue Limits in India:
The Central Insecticides Board and Registration Committee (CIBRC) registers pesticides in India and recommends them for various crops.
A total of 234 pesticides have been registered by CIBRC (including Endosulfan* the use of which was banned in India in May 2011).
Food Safety and Standard Authority of India (FSSAI) is responsible for setting MRLs for the pesticides that have been registered by CIBRC.
The MRLs for all registered pesticides should be set for all the crops they have been registered.
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.
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 slide contains introduction about pesticide, steps involved in pesticide analysis and different methods for estimation of pesticide residue in milk.
Presented by: G.Hima Bindu (Deparment of pharmaceutical analysis),
RIPER,anantapur.
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 Methods of Detection of Natural, Permitted and Non Permitted Dyes.
Presented by: P.SUDHEER KUMAR (Department of pharmaceutical analysis).
RIPER, anantapur
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 I have given brief knowledge about types of preservatives. This slide is recommended to students who are new to this particular topic or those who want notes for examination. I hope you will get benefit from this slide. Do comment for any improvement or want slides that i should prepare for you.
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
In this slide contains Determination of heavy metals, fineness of powder, density and moisture.
Presented by: Malarvannan M (Department of pharmaceutical analysis).RIPER, anantapur
In this slide contains introduction and various methods for analysis of milk.
Presented by: KHALID KUWAITY (Department of pharmaceutical analysis).
RIPER, anantapur
TLC for chlorinated pesticide determination Bapi Mondal Bapi Mondal
In this assignment file i will demonstrate the process involved in Thin layer chromatography for Chlorinated Pesticide
determination. if u like this work feel free to share this file. thank you.
Estimation of total sugars, Extration, Total sugar introduction, estimation, principle, materials required, procedure, calculation , result , observation , colorimetry, calibration curve, important note, videolinks.
In this slide contains Quality control test and Analysis of Wine and Beer.
Presented by: SHAIK GOUSE UL AZAM (Department of pharmaceutical analysis ).
RIPER, anantapur
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical aspects of the method, assisting analysts in optimizing their methods for the most challenging analyses.
Introduction to Screening Models Of Anti Cancer Drugs
Need for novel anti cancer drugs, In - vitro methods, In - vivo methods, Advantages and disadvantages
Presented by
T. Niranjan Reddy
Department of Pharmacology
Introduction to Artificial Sweeteners & Method of Analysis, Chemical Structures and Basic Characteristics of Artificial Sweeteners:
Presented by
M.Sudheeshna
Pharmaceutical Analysis
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 slide contains introduction about pesticide, steps involved in pesticide analysis and different methods for estimation of pesticide residue in milk.
Presented by: G.Hima Bindu (Deparment of pharmaceutical analysis),
RIPER,anantapur.
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 Methods of Detection of Natural, Permitted and Non Permitted Dyes.
Presented by: P.SUDHEER KUMAR (Department of pharmaceutical analysis).
RIPER, anantapur
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 I have given brief knowledge about types of preservatives. This slide is recommended to students who are new to this particular topic or those who want notes for examination. I hope you will get benefit from this slide. Do comment for any improvement or want slides that i should prepare for you.
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
In this slide contains Determination of heavy metals, fineness of powder, density and moisture.
Presented by: Malarvannan M (Department of pharmaceutical analysis).RIPER, anantapur
In this slide contains introduction and various methods for analysis of milk.
Presented by: KHALID KUWAITY (Department of pharmaceutical analysis).
RIPER, anantapur
TLC for chlorinated pesticide determination Bapi Mondal Bapi Mondal
In this assignment file i will demonstrate the process involved in Thin layer chromatography for Chlorinated Pesticide
determination. if u like this work feel free to share this file. thank you.
Estimation of total sugars, Extration, Total sugar introduction, estimation, principle, materials required, procedure, calculation , result , observation , colorimetry, calibration curve, important note, videolinks.
In this slide contains Quality control test and Analysis of Wine and Beer.
Presented by: SHAIK GOUSE UL AZAM (Department of pharmaceutical analysis ).
RIPER, anantapur
This webinar will provide pesticides residue analysts with valuable information on the development and optimization of chromatographic separations and mass spectrometry methods for the analysis of pesticide residues in food. The expert speakers will share their knowledge in understanding the critical aspects of the method, assisting analysts in optimizing their methods for the most challenging analyses.
Introduction to Screening Models Of Anti Cancer Drugs
Need for novel anti cancer drugs, In - vitro methods, In - vivo methods, Advantages and disadvantages
Presented by
T. Niranjan Reddy
Department of Pharmacology
Introduction to Artificial Sweeteners & Method of Analysis, Chemical Structures and Basic Characteristics of Artificial Sweeteners:
Presented by
M.Sudheeshna
Pharmaceutical Analysis
in this slides contains method for Herbal Product Standardization and chromatographic technique.
Presented By: G.Aravind Kumar (department of industrial pharmacy).
RIPER, anantapur.
In this slide contains Introductionnof Indian pharmacopeia, ayurvedic, unani pharmacopeia and monographs of herbal drugs.
Presented by: P.SUDHEER KUMAR (Department of pharmaceutical analysis ).RIPER, anantapur
In this slide contains definition and determination of Iodine value, Rancidity, Peroxide value.
Presented by: K. SANDHYA RANI (Department of pharmaceutical analysis).RIPER, anantapur
Target Validation
Introduction,Drug discovery, Target identification and validation, Target validation and techniques
By
Ms. B. Mary Vishali
Department of Pharmacology
Preclinical Development, Introduction
Definition, Stages of development of a new drug, Objectives of Preclinical studies, Several steps in preclinical trials, Types of studies in Preclinical trials, Importance of preclinical trials
By
Ms. I. Sai Reddemma.
Department of Pharmacology
In this slides contains recall classification, strategy, effect of recall system and case study.
Presented by: V.Nabi Rasool. (Department of pharmaceutical analysis and quality assurance)
RIPER, anantapur.
In this slide contains principle, advantage, dis advantage and application of UPLC.
Presented by: P. Sudheer Kumar. (Department of pharmaceutical analysis)
RIPER, anantapur.
In this slide contains the deep explanation of Methods of Determination for Drug-Excipient Compatibility Studies.
Presented by: G.Aravind Kumar (Department of industrial pharmacy),
RIPER, anantapur.
In this slide contains Monographs of herbal drugs: Siddha and Unani pharmacopeia
Presented by: P. VENKATESH (Department of pharmaceutical analysis).RIPER, anantapur
JOURNAL CLUB PRESENTATION (20L81S0402-PA & QA)
Presented by: K VENKATSAI PRASAD (Department of pharmaceutical analysis and quality assurance).RIPER, anantapur
In this slide contains Study of Quality of Raw Materials and General methods of analysis of Raw materials used in cosmetic manufacture as per BSI
Presented by: P.PAVAN KALYAN (Department of pharmaceutical analysis).RIPER, anantapur
In this slide contains Determination of Acid value, Saponification value and Ester value.
Presented by: P.NARESH (Department of pharmaceutical analysis).RIPER, anantapur
A brief information about the SCOP protein database used in bioinformatics.
The Structural Classification of Proteins (SCOP) database is a comprehensive and authoritative resource for the structural and evolutionary relationships of proteins. It provides a detailed and curated classification of protein structures, grouping them into families, superfamilies, and folds based on their structural and sequence similarities.
What is greenhouse gasses and how many gasses are there to affect the Earth.moosaasad1975
What are greenhouse gasses how they affect the earth and its environment what is the future of the environment and earth how the weather and the climate effects.
Richard's aventures in two entangled wonderlandsRichard Gill
Since the loophole-free Bell experiments of 2020 and the Nobel prizes in physics of 2022, critics of Bell's work have retreated to the fortress of super-determinism. Now, super-determinism is a derogatory word - it just means "determinism". Palmer, Hance and Hossenfelder argue that quantum mechanics and determinism are not incompatible, using a sophisticated mathematical construction based on a subtle thinning of allowed states and measurements in quantum mechanics, such that what is left appears to make Bell's argument fail, without altering the empirical predictions of quantum mechanics. I think however that it is a smoke screen, and the slogan "lost in math" comes to my mind. I will discuss some other recent disproofs of Bell's theorem using the language of causality based on causal graphs. Causal thinking is also central to law and justice. I will mention surprising connections to my work on serial killer nurse cases, in particular the Dutch case of Lucia de Berk and the current UK case of Lucy Letby.
Cancer cell metabolism: special Reference to Lactate PathwayAADYARAJPANDEY1
Normal Cell Metabolism:
Cellular respiration describes the series of steps that cells use to break down sugar and other chemicals to get the energy we need to function.
Energy is stored in the bonds of glucose and when glucose is broken down, much of that energy is released.
Cell utilize energy in the form of ATP.
The first step of respiration is called glycolysis. In a series of steps, glycolysis breaks glucose into two smaller molecules - a chemical called pyruvate. A small amount of ATP is formed during this process.
Most healthy cells continue the breakdown in a second process, called the Kreb's cycle. The Kreb's cycle allows cells to “burn” the pyruvates made in glycolysis to get more ATP.
The last step in the breakdown of glucose is called oxidative phosphorylation (Ox-Phos).
It takes place in specialized cell structures called mitochondria. This process produces a large amount of ATP. Importantly, cells need oxygen to complete oxidative phosphorylation.
If a cell completes only glycolysis, only 2 molecules of ATP are made per glucose. However, if the cell completes the entire respiration process (glycolysis - Kreb's - oxidative phosphorylation), about 36 molecules of ATP are created, giving it much more energy to use.
IN CANCER CELL:
Unlike healthy cells that "burn" the entire molecule of sugar to capture a large amount of energy as ATP, cancer cells are wasteful.
Cancer cells only partially break down sugar molecules. They overuse the first step of respiration, glycolysis. They frequently do not complete the second step, oxidative phosphorylation.
This results in only 2 molecules of ATP per each glucose molecule instead of the 36 or so ATPs healthy cells gain. As a result, cancer cells need to use a lot more sugar molecules to get enough energy to survive.
Unlike healthy cells that "burn" the entire molecule of sugar to capture a large amount of energy as ATP, cancer cells are wasteful.
Cancer cells only partially break down sugar molecules. They overuse the first step of respiration, glycolysis. They frequently do not complete the second step, oxidative phosphorylation.
This results in only 2 molecules of ATP per each glucose molecule instead of the 36 or so ATPs healthy cells gain. As a result, cancer cells need to use a lot more sugar molecules to get enough energy to survive.
introduction to WARBERG PHENOMENA:
WARBURG EFFECT Usually, cancer cells are highly glycolytic (glucose addiction) and take up more glucose than do normal cells from outside.
Otto Heinrich Warburg (; 8 October 1883 – 1 August 1970) In 1931 was awarded the Nobel Prize in Physiology for his "discovery of the nature and mode of action of the respiratory enzyme.
WARNBURG EFFECT : cancer cells under aerobic (well-oxygenated) conditions to metabolize glucose to lactate (aerobic glycolysis) is known as the Warburg effect. Warburg made the observation that tumor slices consume glucose and secrete lactate at a higher rate than normal tissues.
Multi-source connectivity as the driver of solar wind variability in the heli...Sérgio Sacani
The ambient solar wind that flls the heliosphere originates from multiple
sources in the solar corona and is highly structured. It is often described
as high-speed, relatively homogeneous, plasma streams from coronal
holes and slow-speed, highly variable, streams whose source regions are
under debate. A key goal of ESA/NASA’s Solar Orbiter mission is to identify
solar wind sources and understand what drives the complexity seen in the
heliosphere. By combining magnetic feld modelling and spectroscopic
techniques with high-resolution observations and measurements, we show
that the solar wind variability detected in situ by Solar Orbiter in March
2022 is driven by spatio-temporal changes in the magnetic connectivity to
multiple sources in the solar atmosphere. The magnetic feld footpoints
connected to the spacecraft moved from the boundaries of a coronal hole
to one active region (12961) and then across to another region (12957). This
is refected in the in situ measurements, which show the transition from fast
to highly Alfvénic then to slow solar wind that is disrupted by the arrival of
a coronal mass ejection. Our results describe solar wind variability at 0.5 au
but are applicable to near-Earth observatories.
Method for estimation of Pesticide in Vegetables (Food analysis)
1. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 1
A Seminar as a part of curricular requirement
for I year M. Pharm I semester
Presented by
M.MALARVANNAN. (20L81S0704).
M.PHARM
Department of Pharmaceutical Analysis.
Under the guidance/Mentorship of
Dr. P. Ramalingam., Ph.D.
Director- R&D Division,
Professor of pharmaceutical analysis
and medicinal chemistry
METHODS FOR ESTIMATION OF
PESTICIDES IN VEGETABLES
2. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 2
S.NO CONTENT
1 Introduction
2 Colour code for different pesticide
3 Regulation
4 Terminology
5 Work flow for analysis of pesticide residue
6 Sample collection
7 Sample preparation
8 Extraction of vegetable sample
9 Multiresidue method for determination of Organophosphorus
pesticide.
10 Multiresidue method for determination of chlorinated pesticide.
11 Reference
Content Table
3. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 3
Pest:
• Pest is any Animal, Plant, or Microorganism that causes trouble,
injuries or destruction of plant or crops.
Pesticide:
• The FAO defines pesticide as any substance intended for preventing,
destroying, repelling, attracting any pest including harm.
Main classes of pesticides:
Introduction
Herbicide Fungicide
Insecticide Rodenticide
4. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 4
Effect of pests and insects on various foods:
Damage to existing crops.
Damage the crops during storage.
Damage the food products.
Damage the fresh foods like vegetables and fruits.
Eg: Onion, tomato, apple etc..
Damage the milk and milk products.
Eg: Cheese, butter, cream etc..
5. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 5
Colour code for different pesticide
LABLE LEVEL OF TOXICITY LD50 CHEMICALS
Extremely toxic 1-50
Monocritophos, Zinc
phosphate, Ethyl mercury
acetate.
Highly toxic 51-500
Endosulfan, Carbaryl,
Quinalphos.
Moderately toxic 501-5000
Malathion, Thiram,
Glyphosate.
Slightly toxic More then 5000
mancozeb, Oxyfluorfen,
mosquito repellant oils
and liquids.
6. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 6
a). Chlorinated pesticides:
b).Organo-Phosphorus pesticides:
Chemical classification of pesticide
ENDOSULFAN HEPTACHLOR
DDT
ACEPHATE MALATHION
ETHION
7. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 7
C). Synthetic pyrethroids :
d). Thiazole Fungicide:
Continued…
FLUVALINATE
FENOPROPATHRIN CYHALOTHRIN
HEXACONAZOLE
PROPICONAZOLE MYCLOBUTANIL
8. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 8
• It was considered that the ultimate goal in fair practice in
international trade depended, among other things, on the reliability
of analytical results.
• Particularly in pesticide residue analysis, depended not only on the
availability of reliable analytical methods.
• But also on the experience of the analyst and on the maintenance of
good practice in the analysis of pesticides.
• It contains three inter-related parts
The Analyst
Basic Resources
The Analysis
Analysis of pesticides
9. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 9
• Each country adopts their own agriculture policies like Maximum
Residue Limits (MRL) and Acceptance Daily Intake (ADI).
• Some countries use the international maximum residue limits –
codex Alimentarius to define the residue limits.
• This was established by Food and Agriculture Organisation of the
United Nations (FAO) and Would health organisation (WHO) in 1963
to develop international food standard.
• “Codex India” the national codex contact point (NCCP) for India
Regulation
10. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 10
• Pesticide residue: Any specific substance in food, commodities or
animal feed resulting from the use of pesticide.
• Maximum residual limit (MRL): The limit beyond which pesticide
levels are not legally permitted.
• Acceptance daily intake (ADI): It is the daily dose of chemical
which during an entire life time, appears to be without appreciable
risk on the basis of all facts known at that time.
• lowest Calibrated level (LCL): The methods with sufficient
sensitivity to determine residues at levels two or more orders of
magnitude lower.
• Persistence: The chemical that remain active for a long period of
time after application.
Terminology
11. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 11
Central codex committee of food standards
(The prevention of food adulteration Act,1954)
Maximum Residue Limit in India
PESTICIDE FOOD MRL (mg/kg)
Dithiocarbamates Tomatoes 3.0
Benomyl Fruits
Vegetables
1.0
0.50
Captafol Tomato 5.0
Copper oxychloride Fruits and vegetables 20
carbendazim Fruits
Vegetable
5.0
0.50
Profenfos cabbage, onion, tomato. 0.05
chlorothalonil Potato 0.1
captan Fruits and vegetables 15.0
12. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 12
PESTICIDE FOOD MRL (mg/kg)
Dodine Apple 5.0
Penconazole Grapes 0.2
Tricyclazole Rice 0.02
Myclobutanil Grapes 1.0
Dimethoate Carrot, onion, cucumber. 0.02
Propiconazole Wheat 0.05
Malathion Tomato, onion. 3.0
Endosulfan Tomato 0.5
Continued….
13. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 13
Sampling
Sample
Preparation
Sample Analysis
Data
evaluation
and
Reporting
Workflow for analysis of pesticide
Residue
14. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 14
Sample collection
COMMODITY EXAMPLES MINIMUM QUANTITY
REQUIRED
Small or light products, unit
barries weight upto about 25 g
Peas, olives parsley 1 kg
Medium sized products unit
weight usually between 25 to
250g
apples, oranges, carrots
potatoes
1 kg
(at least 10 units)
Large sized products unit
weight over 250 g
cabbage, melons, cucumber 2 kg
(at least 5 units)
Dairy products Whole milk, cheese
Butter , cream
0.5 kg
Egg (10 unit if whole) meat Poultry, fat, fish and other
fish and animal products
NA
Oils and fats cottonseed oil margarine 0.5 kg
Cereals and cereal products NA 0.5kg- 1 kg
Spices Chilies, cumin, coriander 0.25kg
15. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 15
• The well-equipped food analysis laboratory should have a variety of
sample preparation equipment including mechanical choppers,
mincers, grinders, blenders and a hammer or similar mill.
• Generally the vegetables are moist food category so it can be
chopped or minced.
Chopper grinder
Sample preparation
Mincer
16. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 16
Homogenization of sample composite:
• Ideally, the entire sample should be homogenized using
equipment such as a Hobart food cutter.
• Before being placed in the chopper, samples may need to be
either halved or quartered or cut into small (5-10 cm) pieces. After
homogenization, remove a portion for analysis.
• Pesticides may tend to collect in top of vegetables.
• If the homogenized sample is not immediately
analysed, store it in a clean container with a
tight closure and freeze.
17. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 17
• Normally the whole sample is stored depending analysis at <-10 °C.
• Homogenization will increase the rate of enzymatic hydrolysis so
frozen homogenized samples should be analysed within two weeks.
• In vegetables the edible portion is analysed.
• Soil will be removed from root vegetables, by gentle brushing under
a stream of water and Outer leaves of cabbage, cauliflower, etc. will
be removed.
Sample storage
SAMPLE TYPE STORAGE
Dry feed Room temperature in airtight container
Fruits and vegetables Refrigerate the whole sample
Feeds for fumigant analysis seal in plastic bags and freeze
18. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 18
Storage of primary standards:
• Proper storage of reference standards in order to maximize
preservation of chemical integrity is an essential part of the
analytical process.
• Small sample vessels, air-tight container, moisture-free atmosphere.
large, wide mouth, resealable glass jars loaded with 2 to 4 cm of an
appropriate desiccant.
Solvents:
• Toluene, Iso-octane (2,2,4-trimethylpentane), ethyl acetate and
hexane. All solvents should be pesticide grade and distilled-in glass.
Pesticide standards
19. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 19
a) Preparation of stock solution 1 mg/mL (1000 ppm)
• Weigh 50 mg of the pesticide of pesticide reference standard and
transfer to 50 mL volumetric flask. Dissolve the pesticide in a suitable
solvent and make to volume.
b) Intermediate solution 10 µg/mL (10 ppm)
• Pipet 1 mL of the stock solution into individual 100 mL volumetric
flask. Dilute to volume with the suitable solvent.
c) Working solution 1 µg/mL (1 ppm)
• Pipet 10 mL of the intermediate solution into 100 mL volumetric
flask. Dilute to volume with the suitable solution.
Preparation of standard solution of pesticides:
20. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 20
The vegetables are covered under the Group-Ⅰcategory.
The Group-Ⅱ&Ⅲ are milk and cereals respectively.
Simple extraction method:
50g of chopped sample is added into high speed blender jar.
100ml of acetone
Blended for 2mins at high speed.
Filter with Buchner funnel.
Washed with 50ml of acetone.
Extract brought to 150-200ml volume with acetone: water (2:1).
Extraction of vegetable sample
21. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 21
a) Extractive method
QuEChERS Method extraction
Marginizing
the
vegetables
materials
Add solvent Shake
vigorously
(vortex)
Add
extraction
salt.
Transfer to
centrifuge
tube
22. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 22
Continued…
Shake
vigorously
(vortex)
And transfer
to centrifuge
for 2mins
23. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 23
b) Clean up method:
• The removal of interfering co- extractives from extract is called clean
up. By using dispersive solid phase extraction (dSPE).
Continued…
Shake
vigorously
(vortex)
And transfer
to centrifuge
for 2mins
Collect the
supernatant
Add
supernatant
in dSPE
sorbent
Transfer to
sample vial
24. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 24
Solid phase extraction cartridges:
• Serves the dual purpose of extraction and clean up. Advantages of
SPE device over other conventional solvent extraction and clean up
of pesticides includes better reproducibility.
Recent Trends in Clean up
25. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 25
GC method:
Multiresidue method for determination
Organophosphorus Pesticide
Column dimensions and type SPB-5 (Supelco, Bellefonte, PA) or any
equivalent, 30 m × 0.53 mm
Carrier gas Nitrogen
Carrier gas pressure 20 psi
Carrier gas Flow 15 mL/min
Injector temperature 220°C
Detector flame photometric detector
Detector temperature 300°C
Initial temperature 140°C, hold 2 min
Final temperature by 140 °C to 240 °C at 5°C/min.
26. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 26
Chromatography clean-up columns:
Read to use Extrelut-3, needle is fixed at column end as flow regulator.
Glass column 30cm x 20cm with glass septum (carbon-celite cleanup).
Reagents:
Reference standard solution: prepared using heptane or n-hexane.
Solvents: acetone, acetonitrile, benzene, methanol, n-hexane (all HPLC grade).
Silanized glass wool.
Active carbon.
Sodium chloride.
Cotton wool washed with acetone and n-hexane.
Continued…
27. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 27
Pesticide standard solution:
Stock solution of 1mg/ml using ethyl acetate.
Working solution of 0.5µg/ml.
Extraction:
50g of chopped sample is added into high speed blender jar.
100ml of acetone
Blended for 2mins at high speed.
Filter with Buchner funnel.
Washed with 50ml of acetone.
Extract brought to 150-200ml volume with acetone: water (2:1).
Continued…
28. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 28
Partition:
25g of sample is placed in a separating funnel.
100ml of dichloromethane, 100ml of acetone and 10gm Nacl is added.
Shake vigorously till most Nacl is dissolved and 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 the organic layers are collected and concentrated just to dryness in rotary
vacuum evaporator
Continued…
29. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 29
Chromatographic column clean up:
Glass column is filled with 2g celite and 4g carbon.
carbon: celite (4:1) is added.
Topped with glass wool plug
Column is washed with 20ml benzene.
Sample is transferred quantitatively with small portion 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 alalyzed by GC.
Determination:
Residue are quantified by height or are measurement from solution of known
concentration of authentic compounds.
Continued…
30. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 30
• Calculation:
• Retention time:
Compound Sample SPB-5
Acephate NA 0.26
Malathione Onion 1.16
Parathione Tomato 1.19
Paraoxon NA 1.06
Ethion NA 1.73
31. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 31
GLC determination:
• For good separation of chlorinated pesticides, a non-polar/fused silicated
quartz capillary column and similar are recommended.
Multiresidue method for determination
Chlorinated Pesticide
Column dimensions and type 30 m × 0.25 or 0.32 mm fused silica capillary column
chemically bonded with SE-54
Carrier gas Helium
Carrier gas pressure 16 psi
Injector temperature 225°C
Detector Electron capture detector
Detector temperature 300°C
Initial temperature 100°C, hold 2 min
Temperature program 100 °C to 160 °C at 15°C/min followed
Final temperature by 160 °C to 270 °C at 5°C/min.
32. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 32
• Calculation:
• Retention time:
Compound Sample SE-54
Aldrin NA 14.70
Dieldrin NA 18.74
Endosulfan 1 Tomato 17.62
Endosulfan II Beetroot 20.11
Heptachlor Brinjal 13.59
33. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 33
Clean up VS Non clean up
34. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 34
Pesticides in spinach sample
35. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 35
100-Compound Pesticide mixture
36. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 36
224-Compound Pesticide mixture
37. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 37
300-Compound Pesticide mixture
38. RIPER
AUTONOMOUS
NAAC &
NBA (UG)
SIRO- DSIR
Raghavendra Institute of Pharmaceutical Education and Research - Autonomous
K.R.Palli Cross, Chiyyedu, Anantapuramu, A. P- 515721 38
1. Joint FAO/WHO Food Standard Programme. “Codex Alimentarius Commission”
Report of the thirty fifth session of the Codex Committee on Pesticide Residues,
2003. pg. 46-55.
2. Joan Stevens, “QuEChERS 101 The basic and beyond” agilent tech slides, 2010.
3. Rohan Dasika, Siddharth Tangirala. “Pesticide residue analysis of fruits and
vegetables” jurnal of environmental chemistry and ecotoxicology Vol.4(2), 2012.
pg 19-28.
4. Application notebook. “Agilent food testing solutions” 2012. pg24-27.
5. Ministry of health and family welfare, govt of India “fassai Manual of methods
of analysis of food pesticide residue” Manual 11. 2015, pg.5-70.
6. Restek “comprehensive solution simplify sample prep and analysis” 2020. pg-5.
7. Manish joshi, “Pesticide residue analysis” www.slideshare.net
Reference