2. PESTICIDE RESIDUES MONITORING IN FOODS >>> OUTLOOK >>> MOHAMED H. EL-SAEID, Ph.D. Chemistry & Pesticide Residue Analysis Chemistry & Pesticide Residue Analysis

3. INTRODUCTION  Several hundreds of Pesticides widely used in the world for agricultural and other purposes such as Parathyroid, Herbicides, Fungicides, Carbamates, OCPs & OPPs…. etc.  Using cause a residues in foods, fruits, vegetables, water, soil & air.  The use of pesticides results in foods as residues, consequently many healthy problems occur in the human food consumption by interact with the human body in different ways of disease & toxic effect.

4. HAZARDOUS  Deaths are estimated to be about 5.000 a year.  Every 17 min. a person die by pesticides poisoning.  Poisoning Effects @ Pyrethroids is a Neurotoxic, Nervous poisoning, Sodium channel closing, Itching, Irritation & burning sensation in the face. @ Herbicides is a decrease Oxygen consumption in tissues, Carbohydrate disturb, ATPs inhibition, Liver, Kidney & Nervous system damage. @ Herbicides is a decrease Oxygen consumption in tissues, Carbohydrate disturb, ATPs inhibition, Liver, Kidney & Nervous system damage. @ Fungicides is a Inhibition Enzymes containing SH & Metal, Allergens, Skin irritation & liver disease.

5. @ Carbamates is a Inhibit Esterase’s & AChE. @ OCPs is a Carcinogenic, Liver damage, Increase in Alkaline Phosphaatase & Aldolase activity, Interact with Drugs & Hormones, damaged of Central Nervous s., Disturb Protein & Lipid functions. @ OPPs is a Inhibit AChE, Acute intoxica- tion symptoms, Eye disease, Respiratory system disease, Gastrointestinal system disease & Central Nervous system disease.

6. What We have to do…..  To protect the food customers>>> >> Discovered the a new, rapid & quick techniques & methodology for pesticide residues. techniques & methodology for pesticide residues.  EXTRACTION  EXTRACTION  Supercritical Fluid Ext. (SFE)  Microwave Solvent Ext. (MSE) *  Accelerated solvent Ext. (ASE) *  Sonication Ext. (SAE) *  Solid Phase Ext. (SPE) *  Pressurized Solvent Ext. (PSE) *  Purge trap & Purge Headspace *(EPA & FDA) *(EPA & FDA)

7. SFE & MSE has Potential advantages than conventional extraction. Methods. Potential advantages than conventional extraction. Methods. Reduced time. Reduced time. Superior recovery. Superior recovery. Reduction in solvent usage. Reduction in solvent usage. No cleanup. No cleanup. Safe. Safe. SFE can be coupled directly with SFC. SFE can be coupled directly with SFC. MSE has proven to be safe alternative to conventional organic solvent extraction. MSE has proven to be safe alternative to conventional organic solvent extraction. High ability as Food and soil extraction techniques. High ability as Food and soil extraction techniques.

8. SFEMSE  No cleanup Need for both extraction methods.

9. ASE

10. SPE

11.  DETERMINATION  Supercritical Fluid Chromatography (SFC)  GC-ECD/NPD/FID/FPD HPLC-UV/FL*  Capillary Electro Chromatography (CEC)  ELISA*  LC/MS & LC-MS/MS*  GC-MS & GC-MS/MS* *(EPA, FDA & AOAC )

12. SFC Separation techniques used critical points & carrier gases of CO 2 With modifiers. Separation techniques used critical points & carrier gases of CO 2 With modifiers. CO 2 is a safe gas to use. CO 2 is a safe gas to use. Become increasingly apparent in last several years. Become increasingly apparent in last several years. Complements GC & HPLC, it can be analyze different molecular weights without drivatization. Complements GC & HPLC, it can be analyze different molecular weights without drivatization. Increase the analysis speed 10 times. Increase the analysis speed 10 times. Wider range of detectors, polarity & sensit. Wider range of detectors, polarity & sensit. Can be coupled with SFE for many groups of pesticides residues. Can be coupled with SFE for many groups of pesticides residues. Highly sensitivity. Highly sensitivity.

14. SFC

15. Enzyme Linked Immunosorbent Assay {ELISA} is The EnviroGard Plate Kit is a quantitative laboratory test for the detection of pesticide residues in water, soil and foods uses polyclonal antibodies which bind Ps-enzyme conjugate for a limited number of antibody binding sites inside of the wells. The EnviroGard Plate Kit is a quantitative laboratory test for the detection of pesticide residues in water, soil and foods uses polyclonal antibodies which bind Ps-enzyme conjugate for a limited number of antibody binding sites inside of the wells. EPA, FDA, AOAC and Codex methods. EPA, FDA, AOAC and Codex methods. Rapid (less than 55 min.) for 84 samples. Rapid (less than 55 min.) for 84 samples. Inexpensive, portable & can be used to evaluate many samples at the same time. Inexpensive, portable & can be used to evaluate many samples at the same time. Simple & sensitive (0.001 ppb). Simple & sensitive (0.001 ppb). No solvent disposal. No solvent disposal.

16. Plate Mechanism Plate Mechanism

17. FACTS DETERMINATION DETERMINATION By modified SFC/UVD new techniques can be determined 8 Pyrethroids, 8 Herbicides, 7 Fungicides, 12 Carbamates in 25, 10, 12 & 30 min only. By modified SFC/UVD new techniques can be determined 8 Pyrethroids, 8 Herbicides, 7 Fungicides, 12 Carbamates in 25, 10, 12 & 30 min only. By modified HPLC/FD technique can be determined 8 Carbamates in 55min. By modified HPLC/FD technique can be determined 8 Carbamates in 55min. By modified GC/ECD new techniques can be determined 16 OCPs in 28 min only. By modified GC/ECD new techniques can be determined 16 OCPs in 28 min only. By modified GC/FPD new techniques can be determined 25 OPPs in 66 min only. By modified GC/FPD new techniques can be determined 25 OPPs in 66 min only. MDL were ranged from 0.0001 – 0.02 ppm. MDL were ranged from 0.0001 – 0.02 ppm.

18. Extraction & Determination Time (min.)  Supercritical Fluid Ext. (SFE) 15.0  Microwave Solvent Ext. (MSE) 5.0  Accelerated solvent Ext. (ASE) 20.0  Sonication Ext. (SAE) 30.0  Solid Phase Ext. (SPE) 15.0  Pressurized Solvent Ext. (PSE) 15.0  Purge trap & Purge Headspace 25.0  SFC 10.0  ELISA 2.0  GCs 30.0  HPLC 50.0  LC/MS 40.0  GC-MS 45.0

19. RECOVERY % 8 Pyrethroids 93-103%. 8 Pyrethroids 93-103%. 8 Herbicides 91-102% 8 Herbicides 91-102% 7 Fungicides 90-107% 7 Fungicides 90-107% 12 Carbamates 92-101% 12 Carbamates 92-101% 8 Carbamates 88-103% 8 Carbamates 88-103% 16 OCPs 96-105% 16 OCPs 96-105% 25 OPPs 97 –106% 25 OPPs 97 –106% AOSC dtermined 19 pesticides from 76 by NT. AOSC dtermined 19 pesticides from 76 by NT.

27. CONCLUSION NEW EXTRACTION METHODOLOGY BY SFE, ASE, SONICATION, SPE &MSE WAS SUCCESSFUL FOR MORE THAN 74 PESTICIDE RESIDUES IN FOODS. NEW DETERMIATION METHODOLOGY BY SFC, HPLC& GC WAS SUCCESSFUL FOR 76 PESTICIDE RESID UES IN FOODS. APPLICATION OF NEW METHODOLOGY OBTAINED TO PROTECT THE FOOD CUSTOMERS. ELISA technique coupled with SFE & MSE is less time consuming, high recovery% and more sensitive with lower detection limit of Pesticide residues in foods.

28. RECOMENDATIONS MODERN UNITS AND LABS WITH NEW TECH. FOR MODERN UNITS AND LABS WITH NEW TECH. FOR » RESEARCHES » DATA BASE » MARKETS ( FOODS, WATERS, SOILS……etc. SOILS……etc. » ANALYTICAL QC/QA ACCRED. » PESTICIDE RESIDUE MAPS.

29. PESTICIDE RESIDUES MAPS 1 3 4 5 2

30. >>>>>

31. >>> DDTs >>>

32. >>>>..... فالطير يرقص مذبوحا من شدة الألم..... فالطير يرقص مذبوحا من شدة الألم