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Perfluorooctanoate and Perfluorooctane Sulfonate Concentrations in Surface Water in Japan

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Perfluorooctanoate and Perfluorooctane Sulfonate Concentrations in Surface Water in Japan Journal of J Occup Health 2004; 46: 49–59 Occupational Health Perfluorooctanoate and Perfluorooctane Sulfonate Concentrations in Surface Water in Japan Norimitsu SAITO1, Kouji HARADA2, Kayoko INOUE2, Kazuaki SASAKI1, Takeo YOSHINAGA2 and Akio KOIZUMI2 1Research Institute for Environmental Sciences and Public Health of Iwate Prefecture and 2Department of Health and Environmental Sciences, Kyoto University Graduate School of Medicine, Japan Abstract: Perfluorooctanoate and Perfluorooctane exposed to PFOA through drinking water ingestion. Sulfonate Concentrations in Surface Water in (J Occup Health 2004; 46: 49–59) Japan: Norimitsu SAITO, et al. Institute for Environmental Sciences and Public Health of Iwate Key words: PFOA, PFOS, Surface water, Osaka area, Prefecture—Perfluorooctanoate (PFOA) and Drinking water contamination perfluorooctane sulfonate (PFOS) are synthetic surfactants used in Japan. An epidemiological study Perfluorooctanoate (PFOA) is a synthetic surfactant of workers exposed to PFOA revealed a significant used in a variety of industrial applications1). It is also increase in prostate cancer mortality. A cross-sectional formed through the degradation or metabolism of certain study of PFOA-exposed workers showed that PFOA other manmade fluorochemical products1). perturbs sex hormone homeostasis. We analyzed their PFOA has been reported to cause diverse toxic effects concentrations in surface water samples collected from 2, 3) all over Japan by LC/MS with a solid phase extraction in laboratory animals including primates . An method. The lowest limits of detection (LOD) (ng/L) epidemiological study of workers exposed to PFOA were 0.06 for PFOA and 0.04 for PFOS. The lowest revealed a significant increase in prostate cancer mortality4). limits of quantification (LOQ) (ng/L) were 0.1 for both A cross-sectional study of PFOA-exposed workers showed analytes. The levels [geometric mean (GM); geometric that PFOA perturbs sex hormone homeostasis5), but recent standard deviation (GS)] (ng/L) of PFOA and PFOS in long-term follow-up studies on the workers could not the surface waters were GM (GS): 0.97 (3.06) and 1.19 confirm the earlier adverse effects6–8). (2.44) for Hokkaido-Tohoku (n=16); 2.84(3.56) and 3.69 There is evidence that perfluorooctane sulfonate (PFOS), (3.93) for Kanto (n=14); 2.50 (2.23) and 1.07 (2.36) for which is an analogue chemical of PFOA, is globally Chubu (n=17); 21.5 (2.28) and 5.73 (3.61) for Kinki distributed in humans9, 10) as well as wild life11, 12). In (n=8); 1.51 (2.28) and 1.00 (3.42) for Chugoku (n=9); contrast, contaminations with PFOA have been observed 1.93 (2.40) and 0.89 (3.09) for Kyushu-Shikoku (n=15). 12, 13) The GM of PFOA in Kinki was significantly higher than in wild animals specific to some geographic areas . in other areas (ANOVA p<0.01). Systematic searches Similarly, geographical differences in serum PFOA levels of Yodo and Kanzaki Rivers revealed two highly have been reported in non-occupationally exposed contaminated sites, a public-water-disposal site for persons5, 10). PFOA and an airport for PFOS. The former was Recent ecological investigations have shown that one estimated to release 18 kg of PFOA/d. PFOA in of the ecological sources of PFOA and PFOS is discharge drinking water in Osaka city [40 (1.07) ng/L] was waters from manufacturers14). Moody et al.15) recently significantly higher than in other areas. The present reported that perfluorinated surfactants, including PFOA study confirms that recognizable amounts of PFOA are and PFOS, which were present in some formulations of released in the Osaka area and that people are fire-fighting foams were detected in ground water at U.S. Air Force Bases after cessation of their use. We have also shown that there is a large variation in PFOS contamination Received Sep 2, 2003; Accepted Oct 20, 2003 16) Correspondence to: A.Koizumi, Department of Health and levels in Japan . Geological differences may be attributable 17, 18) Environmental Sciences, Kyoto University Graduate School of to area-specific sources and traffic density . Medicine, 606-8501 Kyoto, Japan The major aims of the present study were twofold. (e-mail: [email protected]) First, the PFOA concentrations were determined in 50 J Occup Health, Vol. 46, 2004 surface water in Japan. This would provide a nationwide Hanshin area (Amagasaki and Kobe cities)], and in profile of the PFOA concentration levels. Since surface Tohoku district (Morioka, Sendai and Yokote cities). To water is the major source of drinking water in Japan, minimize the possibility of sample contamination, information on the concentration levels of surface water containers were thoroughly rinsed with methanol and is important for characterizing the exposure of the deionized water prior to use. Samples were stored at population. The second aim was to find sources of PFOA, room temperature (22°C) prior to analysis. which are associated with geographic differences in PFOA concentration levels. Identified sources would suggest a Field quality samples large industrial production of PFOA or other related A field matrix spike (FMS) and a field matrix blank materials as well as environmental leakages in specific (FMB) were prepared when we collected water samples areas. In the present study, PFOS levels were also in Iwate and Osaka areas. Sixteen samples of two-L determined to delineate differences in the contamination bottles were collected at each sampling site. Eight of the profiles between PFOS and PFOA. sixteen bottles were spiked with analytes for FMS and the other eight bottles were analyzed without spiking for Methods and Materials FMB. FMSs collected in Iwate were spiked with PFOA Standards and PFOS at 1 ng/L in the field. FMSs collected in the Perfluorooctanois acid (98% purity) was obtained from Osaka area were spiked with PFOA at 20 or 200 ng/L Aldrich (Milwaukee, WI) and potassium salt of PFOS and PFOS at 20 ng/L in the field. (98% purity) was obtained from Fluka (Milwaukee, WI). Field spike control samples (FSC), deionized water HPLC-grade methanol was purchased from Wako Pure spiked with amounts of PFOA and PFOS corresponding Chemicals (Osaka, Japan). Presep-C Agri cartridges to the counterpart FMS, were also prepared. We also (Solid phase: Styrene divinylbenzene polymethacrylate prepared deionized water samples without spikes as field on a polyethylene housing) (Presep-C, 220 mg cartridge) blanks. were also purchased from Wako Pure Chemicals (Osaka, Japan). Solid phase extraction Waters including deionized water, were contaminated We split a two-L sample into two one-L preparations. with PFOS16), and deionized water was only used after Individual one-L preparations were processed separately. passage through a Presep-C Agri cartridge to remove the First, they were filtered through glass fiber filters (1.0 residual PFOA and PFOS in this study. We confirmed µmø) (ADVANTEC GA 100, 55 mm ø, ADVANTEC, that the concentration of PFOA or PFOS in the methanol Tokyo, Japan) to remove sediments and biota as used was less than the detection limit. previously reported16). Subsequently, they were passed through a membrane filter (Millipore JAWPO4700, 47 Water sampling mm ø, pore size 1.0 µm)(Millipore, Tokyo, Japan). Water samples were collected from rivers, coastal sea Samples were passed through a Presep-C Agri column at water and tap water. For all sampling, a two-L sample a flow rate of 10 mL/min using a Waters Concentrator was collected in polyethylene terephthalate disposable System (Concentrator Plus, Waters, Tokyo, Japan). containers with narrow-mouth bottle tops and screw caps Presep-C cartridges were then eluted with 1.5 mL of as previously reported (Saito et al.16) We collected tap methanol and concentrated at room temperature under waters in the Osaka area [Kyoto city, Osaka city and nitrogen gas flow to 1 mL for the LC/MS analyses16). Table 1. An optimized analytical condition for PFOA and PFOS by LC/MS HPLC MS Instrument Agilent 1100 Instrument Agilent 1100MSD SL Column Zorbax XDB C-18 (2.1 × 150 mm) Ionization ESI Mobile phase A: CH3CN Nebulizer N2 (50 psig) B: 10 mM CH3COONH4/H2O Drying gas N2 (10.0 L/min, 350°C) Linear gradient; 35%A to 45%A by 2%A/min Polarity Negative Fragmentor 100 V for PFOA and 200 V for PFOS Flow rate 0.2 mL/min. Vcap 4000 V - - Oven temp 40°C SIM (ion) C8F17SO3 : 499, FSO3 : 99 for PFOS - - Injection volume 10.0 µLC7F15CO2 : 413, C7F15 : 369 for PFOA Norimitsu SAITO, et al.: Surface Water Contamination with PFOA and PFOS in Japan 51 Fig. 1. Two typical LC/MS chromatograms of PFOA and PFOS in Iwate Sea water (1 ng/L)(A) and deionized water (0.1 ng/L)(B). - LC/MS and quantification PFOS ion 499 (C8F 17SO3 ) were monitored for The methanol extracts (10 µL injection volume of the quantification. The monitoring revealed a major peak 1 mL extract) were chromatographed by HPLC at a flow with a retention time of 7.4 min for PFOA and 13.3 min rate of 0.2 mL/min as shown in Table 1. The total runtime for PFOS. To avoid interference and ensure complete - was 20 min, without any equilibration time between selectivity, the fragment of PFOA, ion 369 (C7F15 ) and - samples. We employed gradient conditions in the mobile the fragment of PFOS, ion 99 (FSO3 ) were also phase: the concentration of CH3CN (A) in 10 mM monitored. CH3COONH4 buffer (B) started at 35%, then increased Throughout this study, the mean of two one-L to 45% at 2%/min for 5 min, and was then maintained at preparations from a two-L sample was calculated for 45% until 20 min (Table 1). The column temperature quantification of each sampling.
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