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Preliminary National Survey of Dioxin-like Compounds in Oilseed Meals, Fat-soluble Vitamins, Complete Feeds, Milk Products, Minerals, and Wood Products
July 3, 2001 Acting Director, Office of Surveillance and Compliance, HFV-200 Preliminary National Survey of Dioxin-like Compounds in Oilseed Meals, Fat-soluble Vitamins, Complete Feeds, Milk Products, Minerals, and Wood Products FDA District Directors: ATL, BLT, CHI, CIN, DAL, DEN, DET, FLA, KAN, LOS, MIN, NOL, NWE, NYK, PHI, SAN, and SEA Info: FDA District Directors: NWJ and SJN Objective: To determine background levels of dioxin-like compounds in feed ingredients and complete animal feeds. Background: On May 22, 2000, CVM issued an assignment entitled “Preliminary National Survey of Dioxin-like Compounds in Animal Fats, Animal Meals, Oilseed Deodorizer Distillates, and Molasses.” The 5/22/00 assignment looked at the feed ingredients suspected of containing the highest dioxin levels (fish meal, oilseed deodorizer distillates, animal fat, and meat & bone meal). It also looked at ingredients where air deposition (corn), uptake from soil (beet molasses) and fire during the harvest (cane molasses) were likely a major pathway of dioxin contamination. This assignment will be similar to the 5/22/00 assignment, except the Arkansas Regional Laboratory will conduct the analyses and the feed ingredients will be different. The feed ingredients selected in this assignment were considered to be in the second tier regarding likelihood of elevated dioxin levels. CVM realizes it is more of an art than a science when it comes to prioritizing samples for dioxin analysis, but believes it is important to discuss the major reasons why these feeds were selected. There were several factors involved in the selection of complete feed, oilseed meals, fat-soluble vitamins, milk products, mineral products, and wood products. These factors include, but are not limited to, past history of dioxin contamination, the likelihood the ingredient would be used in a ration, the amount typically used in a ration, the percentage fat, the likelihood of having a dioxin contamination from the manufacturing process, the likelihood of having elevated dioxins at the mine of origin of the ingredient, and the need to be able to compare the results from a single ingredient with levels typically found in complete feeds. There is very little information on background levels of dioxins in complete feed. This information will be useful if the FDA has to consider taking regulatory action on an individual feed ingredient or the total ration. Oilseed meals are commonly used at levels greater than 10% of the diet in many animal species. While oilseed meals are primarily utilized for their high levels of crude protein (about 25-50%), they also contain some fat (about 1.5-8.0% depending an whether the fat is solvent or mechanically extracted). The oilseed meals could also potentially pick up dioxins during the manufacturing process or when anti-caking agents are mixed with them. Additional information on dioxins in fat-soluble vitamins (A, D, E and K) is important for the following reasons: 1) the fat-soluble vitamins are commonly added at low levels to most animal diets, 2) dioxins are fat-soluble compounds, and 3) there is a wide diversity in how fat-soluble vitamins are derived. Some of these vitamins are synthesized. Some are derived from plants and some come from animals. While milk and milk products for human consumption have been tested for dioxins by the FDA’s Center for Food Safety and Applied Nutrition, there is little, if any, data on dioxins in milk products used in animal feeds. Dried whole milk should contain a minimum of 26% fat and condensed buttermilk and dried cheese often contain about 15-25% fat. In addition to these “fatty” milk products, there are several milk products (casein, whey, skimmed milk, etc.) with low levels of fat (around 1%). Since dioxins are fat soluble compounds, a slightly greater emphasis will be placed on the “fatty” milk products than on the “non-fatty” ones. The potential concerns with mineral products are two-fold. First, they may be like ball clay and contain high dioxin levels from their mine of origin. Second, the manufacturing process, transport and/or prior use of these mineral products may have introduced some dioxin contamination. The potential concern with wood products (cellulose, lignin, etc.) is that the starting material could have been treated with pentachlorophenol (PCP). PCP was a wood preservative whose uses were greatly curtailed because of its high dioxin contamination. Elevated dioxin levels were recently found in choline chloride from the EU and additional analyses indicated that a carrier, pine sawdust, was the likely source of the contamination. The congener pattern in the pine sawdust was consistent with prior PCP treatment. Characterizing the selected feed ingredients: Complete Feed – By definition in the OP 2001 of AAFCO (page 213), a complete feed is a nutritionally adequate feed for animals other than man; by specific formula is compounded to be fed as the sole ration and is capable of maintaining life and/or promoting production without any additional substance being consumed except water. The goal is to collect two complete feeds each for horses, cattle, swine, poultry and pets. Complete feeds for horses and cattle may be difficult to obtain since these animals are often fed concentrates or supplements separate from the fodder (hay or roughage). Concentrates or supplements for horses and cattle that are capable of maintaining life and/or promoting production without any additional substances being consumed except water and fodder will also be acceptable. Vitamin A and its derivatives belong to a large class of structurally related compounds, termed the retinoids. In addition, ?-carotene, a plant pigment, is converted into vitamin A in tissues and is considered a provitamin. The OP 2001 of AAFCO lists definitions for vitamin A oil, vitamin A acetate, vitamin A palmitate, vitamin A propionate, and carotene. The goal of this survey is to collect one sample of vitamin A and its derivatives and one sample of ?-carotene (beta-carotene). The two most prominent members of the vitamin D group are ergocalciferol (vitamin D2) and cholecalciferol (vitamin D3). Ergocalciferol is derived from a common plant steroid, ergosterol, and is the usual form employed for vitamin D fortification of foods. Cholecalciferol is the form of vitamin D obtained when radiant energy from the sun strikes the skin and converts the precursor 7-dehydrocholesterol into vitamin D3. The goal of this survey is to collect one sample of vitamin D2 and one sample of vitamin D3. At least 8 compounds have been isolated from plant sources that have vitamin E activity and these include ?-, ?-, ?-, and ?-tocopherols and ?-, ?-, ?-, and ?-tocotrienols. ?-tocopherol is the most active form of vitamin E. The only naturally occurring stereoisomers of ?-tocopherol should be designated RRR-?-tocopherol or d-?-tocopherol. The totally synthetic ?-tocopherol should be designated all-rac-?-tocopherol or d,l-?-tocopherol. In the OP 2001 of AAFCO there are definitions for tocopherol, ?-tocopherol acetate, and vitamin E supplement. The goal is to collect two samples of synthetic vitamin E (all-rac- or d,l-?-tocopherol acetate; all-rac- or d,l-?-tocopherol) and two samples of “natural” vitamin E (RRR- or d-?-tocopherol acetate; RRR- or d-?-tocopherol). Trace back may be needed to determine if the vitamin E is of “natural” or synthetic origin. There are 4 forms of vitamin K (K1 or phylloquinone; K2(n) or menaquinone-n; K 2(35) or menquinone-7; and K3 or menadione), but the clinical use of vitamin K is largely limited to vitamins K1 and K3. In feeds, the use of vitamin K3 seems to predominate in practical rations although vitamin K1 has often been used in experimental nutrition studies. In the OP 2001 of AAFCO there are 3 forms of vitamin K3 listed (menadione dimethylpyrimidinol bisulfite, menadione nicotinamide bisulfite, and menadione sodium bisulfite complex), but none for vitamin K1. The goal of this survey is to collect one sample of vitamin K3 and one sample of vitamin K1. If vitamin K1 cannot be readily found, then another sample of vitamin K3 will be collected. The goal under this scenario is to collect two different forms of vitamin K3. Milk Products – There are 30 definitions in the milk products section of the OP 2001 of AAFCO (pages 271-4). The goal of this survey is to emphasize those feed ingredients that are considered high in fat (cheese, dried whole milk, condensed buttermilk, etc.) slightly more than those that are not (casein, whey, skimmed milk, etc.). Thus, we plan to collect 6 samples of “fatty” milk products and 4 samples of “non-fatty” milk samples. Two different types of milk products (“fatty” and “non-fatty”) may be collected from the same facility. Although this is a nationwide survey, the types of samples collected will depend on availability of collection sites and, for a few samples, seasonal variation. The 17 districts involved are scheduled to collect from one to seven samples for dioxin analysis according to the FY 2001 ORA Field Workplan for CP 7371.003 (Feed Contaminants Compliance Program). NWJ and SJN districts are not scheduled to collect any samples, but may be asked to do so if a sample can’t be collected in the originally assigned district. The Field will collect a total of 50 samples. Ten samples each from complete feeds, oilseed meals, fat-soluble vitamins, and milk products, seven mineral products, and three wood products are planned for collection. See attachment A for the specific products to be sampled and their appropriate product codes. Our intent is to obtain samples that reflect animal exposure to dioxins. We recognize the difficulties in sampling at farms. Other facilities, such as feed mills, may be used for sampling; however the feed ingredients there may have already been mixed, combined with other ingredients or otherwise contaminated. Therefore the best sites for sampling may be vitamin/mineral/oilseed/wood product manufacturers and milk processors. A sampling chart (attachment B) identifies the sample types, the selected districts where the particular samples will be collected and the number and type of samples to be collected by district. CVM has made no attempt to provide the names of firms that manufacture, distribute, or sell (MDS) complete feeds since complete feeds (or concentrates/supplements for horses and cattle) should be readily available in each district. CVM also believes that soybean meal, cottonseed meal, peanut meal, and canola meal should be readily available in the assigned districts based on the May 22, 2000 assignment. In attachment C, CVM has provided a limited list of firms that MDS sunflower meal in KAN district and safflower or linseed meal in SEA district. There are numerous ingredients that could serve as the source for the copper, zinc, calcium, phosphorus, magnesium, and iron. CVM does not believe it is productive to try and find several sources for each of these ingredients, but has provided a limited list of firms the MDS these minerals in attachment C. CVM believes that salt blocks (source for sodium) should be readily available in SAN district. CVM prefers that calcium carbonate or ground limestone serve as the source of calcium in KAN district and that magnesium oxide serve as the source of magnesium in PHI district. CVM believes that milk processors should be readily available in each district and encourage investigators to contact the FDA milk specialists in each region if they are having difficulty obtaining appropriate milk-related feed samples. CVM has also provided a limited list of firms that MDS fat-soluble vitamins (A, D, E and K) and wood products (cellulose and lignin). In attachment C, please find a limited list of firms that MDS some of the oilseed meals (linseed, safflower and sunflower), six of the minerals (copper, zinc, phosphorus, calcium, iron and magnesium), the fat soluble-vitamins, and the wood products. The address, telephone number and FEI number for each firm are provided when known. CVM realizes that the list of firms in attachment C is by no means exhaustive, but believe they should serve as a good starting point to try and locate a sample of interest. CVM utilized PODS, the internet, and the 2000 Feedstuffs Reference Issue (July 13, 2000, volume 72, number 29) as the source of the information in attachment C. Please don’t hesitate contacting CVM if having difficulty in locating a sample. We will work with you to try and locate a particular sample in your district and may have to reassign a few samples to other districts. Sample Collection: Before beginning this assignment, each district should choose a person as a District Contact. This person will coordinate and communicate with the FDA investigator(s), the FDA’s Arkansas Regional Laboratory (ARL), and CVM regarding sampling and sample transport and tracking. Each District will submit the name and telephone number of the District Contact to Patsy Gardner, the CVM Coordinator for this project, who will inform Meredith Grahn or John Gridley at ARL. After receiving the names, CVM will hold a teleconference with District Contacts, appropriate district personnel, and ARL to get acquainted, resolve any problems and answer questions. Scientists and officials from the EPA Environmental Chemistry Laboratory and EPA headquarters will be invited to participate in this teleconference. The assignments for sampling will be sent to each district via the Field Accomplishments and Compliance Tracking System (FACTS). Also, the assignment with full instructions and attachments will be sent to the FDA districts and ARL by paper copy. A courtesy copy of the assignment will be sent to the EPA Environmental Chemistry Laboratory and EPA headquarters. ARL will assemble a total of 70 sampling packages. ARL will provide each District Contact with sampling packages equal to the total number of sample collections each district is assigned (attachment B). ARL will also provide each District Contact with one additional sampling package in case of breakage or loss. There are 50 samples to be collected from 17 different districts. This leaves 3 extra sampling packages at ARL in case of breakage or loss at a district or if a district not currently scheduled to collect a sample is asked to do so. The sampling package will contain the following items:
There will be six general types of samples collected—oilseed meals, complete feeds, fat-soluble vitamins, milk products, mineral products and wood products. To minimize the potential for contamination, use only the tools in the kit or, if possible, obtain samples without tools (e.g., sampling from a spigot). We suggest the District Contact or designee review their particular sampling assignment (attachments B and C) soon after receipt, making sure that the sample types selected for your district are available at the identified firms. The District Contact or designee will call prospective firms before the investigator visits and determine that each firm produces or uses the ingredient identified in attachment B. The District Contact or designee will give the investigators the sampling packages and a list of firm(s), by sample type, to visit. Although sampling may occur at the manufacturers and processors, some firms identified may not produce the ingredient(s), the product may be unavailable due to seasonality, or the firm may be too distant. For any of these reasons, the District Contact or designee may want to use feed mills or distributors to obtain samples. If the sample is collected at sites other than the manufacturer or processor, it is important that the ingredient not be combined with any other ingredient(s) when collected (except for the complete feeds). At the feed mills or distributors, make every effort to obtain and record on the c/r the name and address of the manufacturer or processor. The sampling chart (attachment B) identifies the number of samples and sample type(s) each district will collect. All samples should be collected by the district within 45 days after the group teleconference. To avoid contamination of the sample jar keep the cover open only as long as it takes to insert the sample into the jar. When collecting the sample, the investigator should use the gloves and the wide-mouthed, amber glass jars with teflon-lined covers, all of which will be provided by your District Contact or designee. For liquid samples, fill the sample jar approximately 1/2 (50%) to 2/3 (67%) full of the ingredient. For non-liquid samples, fill the sample jar approximately 4/5 (80%) full of the ingredient. If the investigator collects more than one sample at a firm, remember to label each jar with the correct sample type. Put the jar in a zip-lock bag and use bubble wrap and flexible coolant packs to protect the samples in transit. To the greatest extent feasible, maintain samples in the dark and under freezing conditions after collection until shipment to ARL. If a firm wants a sample for their own analysis, provide them with a 702 (b) portion using the second sample jar in the sample package. Collect a copy of the label and shipping receipts, if available. If the investigator has any problems or questions during sampling, call the District Contact or designee, or, if necessary, the CVM Coordinator. The District Contact or designee will receive the samples and package each one with a c/r. If the investigator has already packed the sample, make sure it includes the c/r and is wrapped in a flexible coolant pack using suitable packaging for protection. When ready to ship a sample to the lab, the District Contact or designee will call the ARL Sample Custodian (who will inform the ARL director or designee) and identify the sample and the shipper (Fed Ex, Post Office, UPS, etc.). The District Contacts or designee will keep track of the samples sent to the lab and will try to locate any lost sample. If a sample has been lost or compromised, the District Contact or designee will attempt to have another sample collected. If a sample can’t be collected in the selected district for any reason, the CVM Coordinator will be contacted and another district may be asked to collect the sample. Instructions for District Contacts or designee when shipping samples to ARL (see IOM chapter 4 - Sampling, 454.5, page 161):
Sample Analysis: ARL will maintain samples at a freezing temperature in the dark from the time the samples are received until sample analysis is complete. After sample analysis is completed, ARL will store and/or dispose of the unused portions of the samples. Samples will be analyzed for 7 dioxin, 10 furan, and 7 PCB congeners. Samples will be prepared and analyzed using methods and quality assurance/quality control procedures that generally follow those described in EPA’s Method 1613: Tetra- through octa- chlorinated dioxins and furans by isotope dilution HRGC/HRMS (October 1994, Revision B). For the dioxins and furans, details of the methods and a description of the specific changes made to Method 1613 are detailed in the following publication: Determination of 2,3,7,8-chlorine substituted dibenzo-p-dioxins and –furans at the parts per trillion leves in the United States beef fat using HRGC/HRMS, Analytical Chemistry, Vol. 68, No. 4, 1996. For the 7 co-planar PCB congeners of interest (77, 105, 118, 126, 156, 157 and 169), specific details are described in the following publication: Background contamination by coplanar polychlorinated biphenyls (PCBs) in trace level HRGC/HRMS analytical procedures, Chemosphere, Vol. 34, No. 11, 1997. Extraction procedures will vary depending on the specific matrix, but will generally involve solvent extraction followed by the “clean-up” and analytical procedures described in the methods listed above. Details of the extraction procedures once developed and details of the procedures used to ensure that the glass jars with lids, the collecting tools, and the PVC gloves are dioxin free will be provided by ARL to CVM. Regulatory Activities: Although no regulatory action is anticipated, CVM will coordinate a follow-up with the district(s) if elevated levels of dioxins are detected. If you have any question related to regulatory/enforcement activity please contact John Young, CVM, Division of Compliance. Reporting: If computer transmission by FACTS is unavailable, ARL and the District Contacts may send documents to Patsy Gardner by mail (address below) or fax (301-827-1484). Patsy Gardner As CVM Coordinator for this assignment, Patsy Gardner will receive the following information from the District Contacts and ARL:
CVM will send ARL’s analytical data to the collecting districts. The collecting districts will report their work and time under PAC 71003G. The product codes for this assignment are listed in attachment A. Contacts: CVM Compliance: John Young, HFV-232, 301-594-1791, e-mail - jayoung@cvm.fda.gov
Dan McChesney, Ph.D. PRIORITY: HIGH Estimated completion date for sample collection: September 30, 2001 Attachments: Attachment A: Samples to Collect and their Product Codes
220436
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