1 15 3 Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Title A name given to the resource Alvin L. Young Collection on Agent Orange Description An account of the resource The Alvin L. Young Collection on Agent Orange comprises 120 linear feet and spans the late 1800s to 2005; however, the bulk of the coverage is from the 1960s to the 1980s and there are many undated items. The collection was donated to Special Collections of the National Agricultural Library in 1985 by Dr. Alvin L. Young (1942- ). Dr. Young developed the collection as he conducted extensive research on the military defoliant Agent Orange. The collection is in good condition and includes letters, memoranda, books, reports, press releases, journal and newspaper clippings, field logs and notebooks, newsletters, maps, booklets and pamphlets, photographs, memorabilia, and audiotapes of an interview with Dr. Young. For more about this collection, <a href="/exhibits/speccoll/exhibits/show/alvin-l--young-collection-on-a">view the Agent Orange Exhibit.</a> Text A resource consisting primarily of words for reading. Examples include books, letters, dissertations, poems, newspapers, articles, archives of mailing lists. Note that facsimiles or images of texts are still of the genre Text. Box The box containing the original item. 145 Folder The folder containing the original item. 4180 Series The series number of the original item. Series VI Subseries III Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Creator An entity primarily responsible for making the resource Facchetti, S. A. Balasso C. Fichtner G. Frare A. Leoni C. Mauri M. Vasconi Date A point or period of time associated with an event in the lifecycle of the resource 1985 Title A name given to the resource Studies on the Absorption of TCDD by Some Plant Species Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Title A name given to the resource Alvin L. Young Collection on Agent Orange Description An account of the resource The Alvin L. Young Collection on Agent Orange comprises 120 linear feet and spans the late 1800s to 2005; however, the bulk of the coverage is from the 1960s to the 1980s and there are many undated items. The collection was donated to Special Collections of the National Agricultural Library in 1985 by Dr. Alvin L. Young (1942- ). Dr. Young developed the collection as he conducted extensive research on the military defoliant Agent Orange. The collection is in good condition and includes letters, memoranda, books, reports, press releases, journal and newspaper clippings, field logs and notebooks, newsletters, maps, booklets and pamphlets, photographs, memorabilia, and audiotapes of an interview with Dr. Young. For more about this collection, <a href="/exhibits/speccoll/exhibits/show/alvin-l--young-collection-on-a">view the Agent Orange Exhibit.</a> Text A resource consisting primarily of words for reading. Examples include books, letters, dissertations, poems, newspapers, articles, archives of mailing lists. Note that facsimiles or images of texts are still of the genre Text. Box The box containing the original item. 122 Folder The folder containing the original item. 3378 Series The series number of the original item. Series VI Subseries II Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Creator An entity primarily responsible for making the resource Leoni, A. C. Fichtner G. Frare A. Balasso C. Mauri S. Facchetti Source A related resource from which the described resource is derived Chemosphere Date A point or period of time associated with an event in the lifecycle of the resource 1983 Title A name given to the resource A Neutral Clean-Up Procedure Combined with a High Resolution GC-MS technique for the Detection of the 2,3,7,8-TCDD in Various Vegetal Tissues https://www.nal.usda.gov/exhibits/speccoll/files/original/94f608546e2d2ecca9261f21dfc93ffe.pdf a71d57917394bdd89c03da2bc7e1689b PDF Text Text Item D Number 02373 Author Leoni, A. Corporate Author RBDOrt/ATtlCte Tttto Transcript: A Neutral Clean-Up Procedure Combined with a High Resolution GC-MS technique for the Detection of the 2,3,7,8-TCDD in Various Vegetal Tissues, [1983] Journal/Book Title Year 0000 Month/Day Color D Number of knaps DOSCrfcjtOO NOtOS Was Friday, October 05, 2001 Published in Chemosphere 1 983 1 2(4/5) 493-497 Page 2378 of 2422 �A NEUTRAL CLEAN-UP PROCEDURE COMBINED WITH A HIGH RESOLUTION GC-MS TECHNIQUE FOR THE DETECTION OF THE 2,3,7,8-TCDD IN VARIOUS VEGETAL TISSUES A. Leoni - C. Fichtner - G. Frare - A. Balasso-C. Mauri Lombardy Region Government - Special Office for Seveso - Seveso (Italy) S. Facchetti Radiocheioistry and Nuclear Chemistry Division Commission of the European Communities, Joint Research Centra Ispra Establishment - Ispra (VA) Italy INTRODUCTION A study of methods described in the literature reveals two extraction trends: extraction using organic solvents (i.e. hexane, benzene or hexaneacetone mixtures; and alkaline digestion followed by organic extraction. The literature states that the initial digestion of the sample makes possible sapoRification of the fats and the disaggregation of the organic matrix and the possibly adsorbed TCDD should be more easily extracted. So a variety of ve- getal tissues have been submitted by us to a hot digestion in an aqueous median with KOH at 10%. This resulted in a very suitable procedure for vegetal tissues containing a high percentage of water, but it is unsuitable for application to wissues with a high content of starch (i.e. potatoes, wheat, beans, rice, grains of maize etc.), because heating in an alkaline medium produces irreversible gels. On the contary, these samples are hydrolysed in an a- queous medium with HC1 at 5% and heated for 2 hours. The acid digestion is unsuitable for the vegetal tissues that do not contain starch,however, because the organic matrix cannot be disaggregated. Alkaline digestion can prove difficult with other vegetal tissues(i.e. maize and bean plants) which sometimes fora into an emulsion. Therefore alter- native extraction procedures have been investigated, possibly suitable for any type of vegetal tissues. It was found that an extraction performed first with a polar solvent (aethanol) and then with a non-polar one (ntethylene chloride) was suc-resful with all the species of vegetable tissues thus far tested. METHOD The complete method is given schematically in Figure 1 . It should be noted that further improvements to the purification and separation steps are being considered in order to improve the quality of the extracts and, therefore, �to decrease the sensitivity limit. The following comments can be made on the various analysis steos: " Spi*1"? (2)' a double spiking has been used because with a medium mass-spec- trometric resolution many environmental contaminants can interfere with fragments to the masses chosen for the native TCDD and the internal standards. The correct isotope ratio of molecular ions of the native TCDD, and the intensity ratio for the molecular ions of the labelled TCDD being equal to that expected, give the certainty of quantitative identification of 2,3,7,8 -TCDD. " Extraction (3) : a colourful mixture of products is obtained, with the majority of polar and acid compounds in the hydroalchoclic phase. From 50 grams of fresh vegetal tissues 5-r7 g of residual matrix and about 1.5 g of total organic extract residues are obtained. 1.0 g of this latter residue comes from the hydroalchoolic solution and about 0.5 g from dichloromethane. The alkaline digestion produces a less abundant residue (about 0.5 g) due to the saponification of most of the fats which remain in the aqueous phase. - Silica-gel column (4): the dimensions of this column have been specially chosen to adsorb the polar compounds on its upper part, leading in turn to an improvement in chromatographic separation. Benzene was selected as aiu- ting solvent because of its ability to sclubilize products and because of a distinct separation between polar and non-polar products as clearly shown by TLC plates» Columns having a smaller diameter have sometimes shown obstructions with losses of TCDD. - Multilayer column (5): the elution of this column with petroleum ether introduces an alternative chromatographic separation on silica gel based on the different polarities of the solvents. For example the silica-eel co- lustnsJC4} loaded with extracts of green tissues elutes seme orange-yellow •products (carotene, xanthophyll etc.) which ramain attached to the silica-gel of the multilayer-column (5) when petroleum ether is used. The efficacy of^this "double" chromarographic separation is proved by the slight darkening- of tne Celite/H2S04 mixture placed below the silica-gel of the multilayer, .column . This shows that only a few oxidable compounds are still present. rature The size of cur column differs from that described in the lite- . Since the effectiveness of the purification increases with the contact time between the solurion of the sample and the Celite/H2SC4 mixture, only the quantity of the Celite has been increased. Furthermore �i r the dilution of the eluate of column (4) with the petroleum ether orevents both the quick oxidation of the products and carbonization with possible incorporation of TCDO. - Florisilrand alumina columns (6-?8) : specific tests carried out on the florisil column (6) have confirmed that the size specified in the literature is suitable to our method. However taking into consideration that high quan- tities of waxes, resins, lipids and fatty substances might be present in many vegetal tissues, it is advisable to proceed through a second similar chromatographic step, i.e. use of a nicrccolumn packed with neutral alumit na and florisil (7). packed The final purification is obtained with a microcolumn with basic alumina (8). • * GC-MS measurements (9): gas-chromatography with OV-17 and/or Silar 1OC capillary columns and on-colucm injection technique is used. Simultaneous raass spectrometric measurement (KP£10,000) are performed at masses 320 and 322 for native TCDD and the mass corresponding ion of added labelled TCDD. to the most intense molecular Greater specificity derives from the measure- ment of a third ion for the native TCDD (the molecular ion at n/z 324 or the fragment ion at 257) and from the measurement of the most intense molecular ion of a second differently labelled TCDD. Systematic analyses are performed on control samples free of 2,3,7,3-TCDD (blanks) treated in parallel with the samples examined. RESULTS The step by step recoveries and the sensitivity limit have been evaluated experimentally. .Step by step recoveries: 10 ng of 14-C-TCDD have been added to 50 g of fresh 'vegetal tissues. At about 200 pot we estimated a total recovery of 30^5% which remains approximately constant throughout all the purification and separation steps. Table 1 shows the recoveries so far obtained for various / vegetal tissues. .Sensitivity limit; 1 ng of native TCDD and 5 ng of both 37C1-TCDD and 13CTCDD have been adde to 50g of fresh vegetal tissues (carrots and maize)- free of 2,3,7,8-TCDD. Repetitive test have shown a detection limit of 5?10 p t. �rIGURE 1 WASHING AND/OR SCRAPING OF HYPOGENEOUS PARTS M.ethanol (3x300 nil) Dichloromethane (3x300 ml:) CHOPPING AND SPIKING HOMOGENEI3ATIGN EXTRACTION OF TCDD WITH POLAR AND NGN-POLAR" ORGANIC SOLVENTS ADSORPTION CHROMATCGRAPHY ON SILICA-GEL 5 i 6 MULTILAYER COLUMN ABSORPTION CHROMATOGRAPHY ON FLORISIL ADSORPTION-CHROMATOGRAPKY ON NEUTRAL ALUMINA' AND ADSORPTION CHROMATOGRAPHY ON BASIC ALUMINA HIGH RESOLUTION GC-MS IN MULTI-ION DETECTION MODE -ALL SOLVENTS ARE FOR PESTICIDE ANALYSES Column: 0^ 3 .5 cm Packing: silica-gel g.30 Eluent: benzene 400 ml Column : 0, 3.0 cm ,, Packing (from top) : a,c,e) sodium sulphate 1 cm b) silica gel g.20 7 cm d) Celite g.12-E2504 (4ml) 7 cm Sluent: netroleum ether 40-60 (200 mi) Column: <3«j 1.4 cm Packing: Florisil g.5 Eluents: petroleum ether (70ml) and n-Hexane-CH2Cl2 99:1(40 al) (washing fractions) ; n-Kexane: _CH2Cl2 50:30 (50 ml) Column: 0^ 0.8 cm Packing (from top) Florisil g 5 and neutral Alumina g 1 Eluents: n-Kexane (4x2 ml) and n-Hexane: CC14 30:20 (20 ml) n-Hexar.e : (washing fractions CH?C12 ^ Column: 0^0.3 cm Packing: basic Alumina g 2 Sluents: n-Hexane (4x2 ml) and n-Hexane: CC14 80:20 (20 ml) (washing fractions) ; n-Hexane: CH2C12 50:50 (10 ml) �f TABLE 1. Step by step recoveries in various veaetal tissues ^~~--^^STE?S VEGETALS^^-^^^^ a b CARROT 77 BEAN PLANT 83 c d 79 81 79 79 80 82 a » steps 1?5 b = steps 1-?6 c = steps I*7 MAIZE PLANT WHEAT POTATO 80 77 34 81 - 73 70 71 78 76 75 75 d = conclete analvsis I CONCLUSIONS The clean-up method proposed allows quantitative measurements of the 2,3,7,3TCDD present at a level of 25 ppt in vegetal tissue samples of anv origin. Further developments are under consideration in order to improve the cuality of the extracts and to perform measurements that are net affected by interfering substances at about 1 ppt level. BIBLIOGRAPHY 1) S.Facchetti and A. Laoni, Applications of 'lass Spectrcmetry to Trace Analysis, ISPRA, Italy, 29 Septsr.ber-3 October 1930, S. Facchetti (Zd.)-Elsevier Scientific Publishing Company, Amsterdam 2) A. Cavallaro, G. Bartolozzi, D Carreri, A. Gcrni, L. Luciar.i and G. Villa, Private communication (1979) 3) H.K. Wipf, E. Homberger, N. Neuner, U.S. Ranalder, W. Vetter a-.d J.P. Vuilleumier, Private Communication (1973) � Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Title A name given to the resource Alvin L. Young Collection on Agent Orange Description An account of the resource The Alvin L. Young Collection on Agent Orange comprises 120 linear feet and spans the late 1800s to 2005; however, the bulk of the coverage is from the 1960s to the 1980s and there are many undated items. The collection was donated to Special Collections of the National Agricultural Library in 1985 by Dr. Alvin L. Young (1942- ). Dr. Young developed the collection as he conducted extensive research on the military defoliant Agent Orange. The collection is in good condition and includes letters, memoranda, books, reports, press releases, journal and newspaper clippings, field logs and notebooks, newsletters, maps, booklets and pamphlets, photographs, memorabilia, and audiotapes of an interview with Dr. Young. For more about this collection, <a href="/exhibits/speccoll/exhibits/show/alvin-l--young-collection-on-a">view the Agent Orange Exhibit.</a> Text A resource consisting primarily of words for reading. Examples include books, letters, dissertations, poems, newspapers, articles, archives of mailing lists. Note that facsimiles or images of texts are still of the genre Text. Box The box containing the original item. 094 Folder The folder containing the original item. 2378 Series The series number of the original item. Series IV Subseries IV Dublin Core The Dublin Core metadata element set is common to all Omeka records, including items, files, and collections. For more information see, http://dublincore.org/documents/dces/. Creator An entity primarily responsible for making the resource Leoni, A. C. Fichtner G. Frare A. Balasso C. Mauri S. Facchetti Title A name given to the resource Transcript: A Neutral Clean-Up Procedure Combined with a High Resolution GC-MS technique for the Detection of the 2,3,7,8-TCDD in Various Vegetal Tissues, [1983] Subject The topic of the resource dioxin plant analysis laboratory methods