Herbicides in Pooled Raw Milk in Connecticut

136 Journal of Food Protection, Vol. 54, No. 2, Pages 136-137 (February 1991) Copyright© International Association of Milk, Food and Environmental Sanitarians Herbicides in Pooled Raw Milk in Connecticut HARRY M. PYLYPIW, JR. and LESTER HANKIN* Department of Analytical Chemistry, The Connecticut Agricultural Experiment Station, Box 1106, New Haven, Connecticut 06504 Downloaded from http://meridian.allenpress.com/jfp/article-pdf/54/2/136/1662776/0362-028x-54_2_136.pdf by guest on 29 September 2021 (Received for publication June 29, 1990) ABSTRACT and Drug Administration) (2). Concentrations found of these pesticides were always well below the action level. Pooled raw milk samples collected in Connecticut were Since cows in Connecticut consume quantities of corn analyzed for the herbicides 2,4-D, Atrazine, Simazine, and Alachlor. silage and grass, we investigated milk for the presence of For 2,4-D, 25.6% of the samples had no detectable level, for herbicides used on these feeds. Atrazine 7.7%, and for Alachlor 10.3%. None contained Simaz ine. Concentrations averaged 0.021 ppm for 2,4-D, 0.0075 for MATERIALS AND METHODS Atrazine, and 0.0067 for Alachlor. No sample exceeded the EPA tolerance for any of the herbicides. Analysis was by enzyme immunoassay. A total of 78 samples was collected in Connecticut from milk tank trucks from January to April, 1990 by inspectors of the Dairy Division of the Connecticut Department of Agricul ture. Each sample was from a pooled supply from the tank truck Field corn is a major agricultural crop in Connecticut. and represented from 1 to 7 farms. Samples were refrigerated Herbicides are generally applied in the spring, either pre- when collected and delivered to this laboratory within 24 h. or postemergence, to control weeds (3). Applications of Milk was tested for 2,4-D, Atrazine, Simazine, and Alachlor herbicides is not only labor saving but also limits weed by enzyme immunoassay procedures (5). All milk samples were growth when the field is too wet to be cultivated. Herbi prepared by adding 100 ul of the milk to 9.9 ml of distilled cides used to control weeds in corn are generally Alachlor water. A portion of this diluted milk sample (80 ul) was ana and Atrazine. These are usually used preemergence but lyzed in duplicate along with samples of milk spiked with EPA may be used postemergence when the corn is just above standards of Atrazine, Alachlor, and 2,4-D to eliminate matrix effects. The detection limit for these herbicides is 0.001 ppm. the ground. The crop may be diminished by 50% or more Preparation of the antiserum, antibody tubes, and reagent is described if weed control is not used (10). In late summer the corn by Bushway et al. (5). Confirmation of Atrazine and Alachlor in is harvested, chopped, made into silage, and fed to dairy the milk was by mass spectrometry (MS) using the method of cows. Because these herbicides are slightly soluble in water Huang (8). The MS detection limit for these compounds is 0.001 (6,9), they might migrate from soil to corn and thus from ppm. silage to milk. Herbicides also are used on pasture and hayfields to RESULTS AND DISCUSSION control perennial weeds such as wild garlic and onion that can cause off-odors and off-taste in milk. The herbicide The concentrations of 2,4-D, Atrazine, and Alachlor 2,4-D (2,4-dichlorophenoxyacetic acid) is registered for such found are listed in Table 1. No samples were found to uses with a 7-14 d delay in grazing and up to 30 d delay contain Simazine. Many samples had nondetectable levels. in harvesting for hay depending on the formulation. Thus, For 2,4-D, 25.6% of the samples had no detectable amount, milk from cows grazing the pasture or consuming cut grass for Atrazine 7.7%, and for Alachlor 10.3%. might also contain traces of 2,4-D. The concentration of 2,4-D ranged from none detected For many years this laboratory has tested raw milk for to 0.10 ppm with an average for all samples of 0.021 ppm. pesticides using a multi-residue method (4) which essen The average concentration of Atrazine found was 0.0075 tially monitors for chlorinated and organophosphate pesti ppm with a range from 0.001 to 0.019 ppm and for Alachlor cides. Generally, the only pesticide found was DDE the average was 0.0067 ppm with a range from 0.001 to (dichlordiphenyldichloroethylene) and always well below 0.018 ppm. The EPA tolerance concentration is 0.10 ppm the tolerances established at that time by the EPA (Envi for 2,4-D and 0.020 ppm for the other three herbicides (1). ronmental Protection Agency). After DDT (dichlorodiphen- No sample exceeded the tolerance for any of the herbi yltrichloroethane) and DDE were removed by the EPA cides, but sample no. 64 was at the tolerance level. from the allowable tolerance list (1), an action level of Three samples of milk found to contain Atrazine and 1.25 ppm (fat basis) was established by the FDA (Food 2,4-D were pasteurized both at 64°C for 30 min and at JOURNAL OF FOOD PROTECTION, VOL. 54, FEBRUARY 1991 HERBICIDE IN POOLED RAW MILK 137 TABLE 1. Herbicides in pooled raw milk. 63 " 0.028 0.009 0.005 Herbicide - ppm 64 " 0.100 0.009 0.004 Sample Date 2,4-D Atrazine Alachlor 65 " 0.080 0.007 0.005 Number Collected 66 " 0.080 ND 0.006 1 1/30/90 ND 0.004 0.002 67 4/25/90 0.026 0.004 0.002 2 ND 0.008 0.002 68 " 0.039 0.005 0.005 3 0.006 0.007 ND 69 " ND 0.007 0.009 4 0.040 0.016 ND 70 " ND 0.005 0.007 5 ND 0.003 ND 71 " 0.012 0.004 0.005 6 0.030 0.005 0.003 72 " ND 0.004 0.007 7 0.020 0.006 0.001 73 " 0.023 0.007 0.008 8 0.010 0.007 ND 74 " ND 0.004 0.007 9 0.020 0.004 ND 75 " ND 0.007 0.013 10 ND 0.001 0.001 76 " 0.023 0.012 0.012 11 0.010 0.005 0.002 77 " ND 0.005 0.012 12 ND 0.001 0.001 78 " 0.015 0.004 0.009 Downloaded from http://meridian.allenpress.com/jfp/article-pdf/54/2/136/1662776/0362-028x-54_2_136.pdf by guest on 29 September 2021 13 0.050 0.003 ND Wer age 0.021 0.0075 0.0067 14 0.040 0.007 ND 15 0.050 0.004 0.004 16 0.010 0.005 ND 17 2/21/90 0.020 ND 0.001 18 0.050 ND 0.004 19 0.025 ND 0.007 20 ND 0.005 0.008 76°C for 20 sec. One sample was spiked with these two 21 0.015 0.006 0.009 herbicides and pasteurized in a like manner. The concen 22 0.035 0.006 0.008 tration of these herbicides was not diminished by pasteuri 23 0.050 0.005 0.008 zation, with recoveries of at least 95%. 24 0.055 0.005 0.006 This study has found that low levels of 2,4-D, Atrazine, 25 ND 0.006 0.005 and Alachlor are present in milk but below tolerance levels 26 0.022 0.005 0.008 set by the EPA and below toxicity levels suggested by the 27 0.040 0.005 0.011 FDA (7). The presumed pathway is uptake of these herbi 28 0.048 0.005 0.012 cides by corn and grass and subsequent consumption by 29 0.012 0.006 0.003 the cow. Experiments are now in progress to test this 30 0.075 0.005 0.005 31 3/13/90 ND 0.005 0.009 hypothesis. 32 0.010 0.005 0.009 33 0.019 0.006 0.018 ACKNOWLEDGMENTS 34 0.028 0.005 0.017 35 0.028 0.005 0.017 We thank inspectors of the Department of Agriculture for collecting 36 3/14/90 0.010 0.009 0.012 samples, Laura Rousso for technical assistance, Dr. Lee Huang for confir 37 0.010 0.006 0.012 mation of herbicides by mass spectrometry, and Dr. John Ahrens for helpful discussions about use of herbicides. 38 0.032 0.006 0.011 39 ND 0.017 0.010 40 0.025 0.016 0.014 REFERENCES 41 0.025 0.013 0.011 42 0.025 0.017 0.014 1. Anonymous. 1989. Code of Federal Regulations, Title 40, part 180, 43 ND 0.009 0.011 revised as of July 1. 1989. U.S. Government Printing Office, Washing ton, DC. 44 ND 0.015 0.010 2. Anonymous. 1987. FDA Compliance Policy Guides. Chapter 41-Pes- 45 ND 0.017 0.013 ticides. Food and Drug Administration, Office of Enforcement, Divi 46 0.022 0.013 0.017 sion of Compliance Policy, Washington, DC. 47 4/3/90 0.003 0.013 0.006 3. Anonymous. 1990. New England Chemical Weed Control. Coordi 48 0.009 ND 0.006 nated by P.C. Bhowmik, New England. Specialists of the Cooperative 49 0.008 0.006 0.013 Extension Service. University of Massachusetts, Amherst, MA. 4. Anonymous. 1968. Pesticide Analytical Manual, Vol. 1. Food and 50 0.014 ND 0.012 Drug Administration, Washington, DC.

Load more