Liquid chromatographic assay of tetracyclines in tissues of food-producing animals

A survey of the literature is presented on liquid chromatographic (LC) determination of tetracyclines in plasma, urine, and tissues of food-producing animals. Food Safety and Inspection Service (FSIS) research on tetracyclines during 1973-1984 is discussed, including the thin layer chromatographic qualitative identification method for tissues. Research on development of LC column packings for trace level chromatography of tetracyclines and anhydrotetracyclines is also discussed. Data are shown for recovery, ruggedness testing, and analyst qualification studies on the tentative version of the LC method.     

Antioxidant prenylated flavonoids from propolis collected in Okinawa, Japan

Propolis is a resinous substance collected by honeybees from various plant sources. The composition of propolis depends upon the vegetation at the site of collection. We previously isolated four prenylated flavonoids from propolis collected in Okinawa, Japan. In this study, further fractionation of the extracts of Okinawan propolis resulted in the isolation of a new prenylated flavonoid, prokinawan, and four known compounds. The structure of prokinawan was determined by MS and NMR spectroscopic methods. Furthermore, the antioxidant activity using 1,1-diphenyl-2-picryl-hydrazyl radical scavenging and beta-carotene bleaching systems was investigated. The present study proved that the position of the geranyl or prenyl groups on the flavonoid skeleton plays an important role in exhibiting antioxidant activity.     

土壤及畜禽粪肥中四环素类抗生素固相萃取-高效液相色谱法的优化与初步应用

本研究优化了土壤和有机肥中3 种四环素类抗生素的提取和测定方法。方法经优化后,土壤和有机肥中的抗生素的提取效率达到52%~95%,且分析时间大大缩短。本研究还利用优化方法在天津进行了有机肥和菜地中3 种抗生素残留的初步调查。集约化养殖场的猪、鸡粪便中四环素类抗生素残留状况为: 金霉素（CTC）检出率达到78%,最高残留值达到563.8 mg/kg（干基）; 四环素（TC）和土霉素（OTC）检出率也高达56%,最高值分别达到34.8 mg/kg 和 22.7 mg/kg。在天津销售的几种商品有机肥中同样检测出四环素类抗生素的残留,残留水平与猪粪和鸡粪相当。菜田土壤样品中TCs的总检出率为64%,3.种抗生素中土霉素检出率最低为18%,最高值达到105.6 g/kg（风干基）; 四环素检出率为36%,最高值达到196.7 g/kg; 金霉素检出率为32%,最高值达到477.8 g/kg。在所调查土壤中,温室和大棚土壤TCs的残留水平高于露地土壤。占调查样品 27.3% 的菜田土壤中TCs总量超过欧盟规定的生态安全触发线（100 g/kg）,存在一定的潜在生态风险。     

Aluminum solubility of strongly acidified allophanic Andosols from Kagoshima Prefecture,southern Japan

Abstract

The aluminum solubility of acidified soils both from furrows and under tree canopies of a tea garden was studied using equilibrium experiments in 0.01 mol L^?1 CaCl₂ solution systems. The soils were originally classified as allophanic Andosols. The furrow soils were more severely acidified because of the heavy application of nitrogen fertilizer, especially in the upper soil horizons (pH[H₂O] of 3.6–3.8 in the A1 and 2A2 horizons). These acidified soils were characterized by the dissolution of allophanic materials (allophane, imogolite and allophane-like materials) and by an increase in Al–humus complexes. Ion activity product (IAP) values of the strongly acidified soil horizons were largely undersaturated with respect to imogolite (allophanic clay) or gibbsite. Plots of p(Al³⁺) as a function of pH strongly indicated that Al solubility of the soils was largely controlled by Al–humus complexes, especially in the A1 horizon. In the canopy soils, which were more weakly acidified (pH[H₂O] 4.9–5.0), Al solubility was close to that of gibbsite and allophanic materials, indicating that the solubility is partly controlled by these minerals.     

Review of chromatographic methods for chloramphenicol residues in milk, eggs, and tissues from food-producing animals

Although chloramphenicol is not approved for use in food-producing animals in the United States, this broad spectrum antibiotic has been widely used to treat diseases in such animals including the lactating dairy cow. Extremely low ophthalmologic doses of chloramphenicol are known to cause aplastic anemia in humans. The residues in meat, milk, and eggs intended for human consumption cause particular public health concern because the bone marrow aplasia is not dose dependent. Furthermore, chloramphenicol, a known inhibitor of protein synthesis, also retards erythropoiesis, a condition that is dose dependent and may cause allergic hypersensitivity reactions. This paper is a review of sensitive methods that use gas, liquid, thin layer, and simple column chromatography as both determinative and cleanup steps for detecting and quantitating chloramphenicol in edible animal tissues, milk, and eggs.     

Chemical and mineralogical studies on the citrus soils in Wakayama Prefecture,Japan

Wakayama Prefecture is one of the important districts of citrus production in Japan. The citrus groves are located in the northern districts of the prefecture along the watershed of the Kii, and Arita rivers. Geologically, the rocks in these districts are classified into crystalline schist, Palaeozoic Upper Chichibu and Mesozoic Cretaceous systems. The associated soils are chiefly members of the Red Yellow Podzolic and Lithosol group.⁷⁾     

Long-Term Observation of Fogwater Composition at two Mountainous Sites in Gunma Prefecture, Japan

We made serial observations on acid fog at Mt. Akagi and Mt. Haruna, Japan for 5 years. The altitudes of the sampling sites were 1500 m (Mt. Akagi) and 1200 m (Mt. Haruna) above sea level, and the sites were approximately 30 km apart. The average liquid water content (LWC) at Mt. Akagi and Mt. Haruna was 74 mg m^?3 and 63 mg m^?3, respectively. The pH of fogwater was 2.72–7.14 (mean 3.71) at Mt. Akagi and 2.94–6.58 (mean 3.73) at Mt. Haruna. Our long-term observations indicate that there was no significant difference in the chemical components in fogwater at both sites except for ammonium ion. However, there were some cases where the chemical components of fogwater at each site were differed remarkably even in the concurrent fog event. Nitrate and sulfate ions contributed to acidification of fogwater at Mts. Akagi and Haruna and 95% of sulfate ion in the fogwater originated from air pollution. Ammonia gas in the air was the main neutralizer of acidity in fogwater. When absorption of excessive nitric acid gas over ammonia gas in the air occurred, the pH of fogwater was lowered. Our back trajectory analysis indicated that the fogwater at Mt. Akagi was mainly affected by an air mass from the Kanto Plain, including Tokyo, while the fogwater at Mt. Haruna was influenced by an air mass from large, western cities, such as Nagoya and Osaka, as well as Tokyo.     

Influence of Acid Deposition on Inland Water Chemistry - A Case Study from Hyogo Prefecture, Japan -

The Influence of acid deposition on stream and lake water chemistry was studied in a forested watershed of Hyogo prefecture, Japan. Monthly sampling of four streams, one artificial lake, and precipitation was carried out from 1995 to 2000. The pH of the monthly bulk precipitation and rainwater were ranged from 4.06 to 7.10. No trends were evident during the monitoring periods. The pH and alkalinity in the four streams, which flow into the artificial lake, ranged from 6.37 to 8.72 and 0.077 meqL^?1 to 0.485 meqL^?1, respectively. The differences in the water quality of the four streams were related to the geology of each watershed. Lower pH and alkalinity were observed during high- discharge periods. On the other hand, the pH and alkalinity of the outflow from the lake ranged from 6.47 to 7.36 and 0.195 meqL^?1 to 0.339 meqL^?1, respectively. No acidification of the aquatic environment was observed during the investigated periods. The results suggest that this forested ecosystem has the capacity to neutralize incoming acid deposition.     

An analytical survey of aflatoxins in tissues from swine grown in regions reporting 1988 aflatoxin-contaminated corn.

A joint project was undertaken by the Food Safety and Inspection Service (FSIS) and the Agriculture Research Service branches of the U.S. Department of Agriculture to determine the presence of aflatoxins in the U.S. meat supply during a drought year. In 1988, high incidences of aflatoxins occurred in corn grown in regions of the Midwest, Southeast, and South. Six states were identified as having serious aflatoxin contamination in their corn crop: Virginia, North and South Carolina, Texas, Iowa, and Illinois. Swine liver and pillars of diaphragm (muscle) tissues were sampled by federal FSIS Inspectors in plants located in these states. A worstcase sampling plan was conducted. Samples were taken in January 1989 from hogs fed corn soon after harvest and in April 1989 from hogs fed corn originally stored and then fed in the spring. A modification of the official AOAC method for the thin-layer chromatography (TLC) determination of aflatoxins in animal tissue was used to permit quantitation by LC with fluorescence detection. The official AOAC TLC confirmation of identity method was used to confirm all positive samples with B1 concentrations greater than 0.04 ppb and M1 concentrations greater than 0.1 ppb. Sixty samples in the January group and 100 samples in the April group were assayed. Concentrations of aflatoxins B1 and M1 in the first group of pig livers ranged from 0.04 to 0.06 ppb. The identity of aflatoxin B1 was confirmed in all positive samples. Aflatoxin M1 could not be confirmed in any of the positive liver samples because the method was insufficiently sensitive for this aflatoxin.(ABSTRACT TRUNCATED AT 250 WORDS)     

Multielement concentrations in liver and kidney tissues from five species of Canadian slaughter animals

The present paper describes results of a national survey conducted between 1982 and 1989 to determine residues of arsenic, cadmium, copper, mercury, lead, selenium, and zinc in Canadian slaughter animals. Liver and kidney tissues from cattle, swine, poultry, horses, calves, and sheep were tested. Arsenic was found in most avian and porcine samples, and their respective means of 0.36 and 0.26 micrograms/g in liver were 7 to 12 times higher than mean concentrations found in the other species. Cadmium was found in the tissues of all species; however, levels were consistently highest in equine samples with mean values of 3.09 and 27.7 micrograms/g in liver and kidney, respectively. Copper levels greater than 150 micrograms/g were found predominantly in liver from calves and sheep, with values considerably lower in the remaining species. Mercury levels were low or not detected in all species except horses. Ninety % of equine kidneys and 54% of equine livers had mercury concentrations greater than 0.01 microgram/g, with mean values of 0.18 and 0.06 microgram/g, respectively. Lead was found in tissues of all species; however, values greater than 2 micrograms/g were found only in 2 kidneys from adult cattle and 1 kidney from a horse. Selenium, tested only in cattle, was found at mean concentrations of 0.28 microgram/g in liver, and 0.92 microgram/g in kidney. Relatively high zinc levels were found in livers of horses, pigs, and calves, with respective mean concentrations of 67.3, 65.6, and 70.2 micrograms/g.     

Formaldehyde Concentrations in Ambient Air in Urban and Rural Areas in Gunma Prefecture, Japan

We measured formaldehyde concentrations in ambient air at urban (Isesaki) and rural (Annaka) sites in Gunma Prefecture, Japan from June 1998 to March 2003. Measurements were carried out once in a month to obtain daily mean formaldehyde concentrations. At both the sites, mean concentrations of formaldehyde were significantly higher from April to September (summer) than from October to March (winter). Formaldehyde concentrations in Annaka were essentially as high as those in Isesaki in summer, but were significantly lower in winter. At both the sites, concentrations of formaldehyde and oxidants correlated significantly with one another in the summer; correlation coefficients in Annaka and Isesaki were 0.82 and 0.64, respectively. The fraction of formaldehyde formed photochemically based on concentrations of benzene was calculated to be as high as 80% in both the sites in summer. The results suggested that formaldehyde concentrations were high even in rural air, reflecting photochemical reactions rather than automobile exhaust.     

Small-scale survey on the contamination status of butyltin compounds in seafoods collected from seven Chinese cities

Tributyltin (TBT) and its degradation products, dibutyltin (DBT) and monobutyltin (MBT), in the commercial sea products collected from seven Chinese cities were measured to evaluate the extent of contamination and the potential adverse effect on health. Universal existence of butyltins was found in these samples, and the concentrations of TBT ranged from <6.9 to 17175 ng of Sn g(-1) of wet weight. The accumulation ratios of the pollutant in these organisms were as high as 10(3) or more compared with the previously reported data in corresponding water. The existing different accumulation capabilities of pollutants among the various seafood species were studied. It was observed that the butyltin compounds were comparatively stable during cooking or processing procedures in the manner of usual Chinese cooking way. The occurrence of butyltin compounds in sea products indicated a potential danger for the health of people who consumed seafood in these areas.     

Pedogenic characteristics of soils distributed under Warm-temperate forest climate in Nyu mountains,Fukui Prefecture,Central Japan

The bioclimatic conditions, profile morphology and physico-chemical properties of five different soils under the Warm-temperate deciduous broad-leaved forest climate, Warm-temperate lucidophyllous forest climate, and Cool-temperate deciduous broad-leaved forest climate in the northern part of the Nyu mountains in Fukui Pref., Central Japan were examined. The outline of the results is as follows: 1) The Dark red soil, Kunimidake series, derived from pyroxene andesite may have been formed by the hydrothermal action of volcanism. 2) The Dry brown forest soil, Takasu-1 series, showed a brighter colour in the Bw horizon and a sudden decrease in the humus content below the AB horizon, suggesting that this soil was similar to Yellow-Brown Forest soils rather than to Brown Forest soils. 3) The Dry brown forest soil (reddish), Tega series, is likely to be a Yellow-Brown Forest soil derived from the loess which covered the underlying paleo-red soil. 4) The Red soil, Oshibayama series, was a paleo-red soil in which the upper part had been lost by erosion. 5) The Yellow soil, Yada series, on the Takasu coastal terrace was also considered to be a Yellow-Brown Forest soil affected by the seawater components from the neighboring coast. 6) It was suggested that zonal soils formed under the Warm-temperate deciduous broad-leaved forest climate in the northern part of the Nyu mountains, in the northwestern region of Fukui Pref. were Yellow-Brown Forest soils like those under the Warm-temperate lucidophyllous forest climate.     

Limited survey of deoxynivalenol in wheat and corn in the United States

A limited survey was conducted over a 2-year period to determine the incidence and levels of deoxynivalenol (DON) in corn and wheat grown in selected areas of the United States. Samples of corn (198) and wheat (247) were collected and analyzed by a gas chromatographic method. Sixty-six percent of the corn samples collected in 1984 and 30% of the corn samples collected in 1985 contained DON. The average concentration of DON in corn, by state, ranged from 0.11 to 1.20 micrograms/g; the maximum concentration was 2.47 micrograms/g. Only 2 of the 247 samples of wheat contained DON at a concentration greater than 2 micrograms/g, which is the level of concern suggested by the Food and Drug Administration for wheat entering the milling process for human consumption.     

Seasonal and Spatial Variations in the Chemical and Sulfur Isotopic Composition of Acid Deposition in Niigata Prefecture, Japan

The following measurements were carried out to clarify acid deposition in Niigata Prefecture, an area facing to the Sea of Japan. 1) Acid deposition fluxes and sulfur isotopic ratios of atmospheric deposition were measured at 9 sites in the prefecture in 1999. 2) Atmospheric deposition was collected daily at one site in 1997, to measure the sulfur isotopic variations of sulfate together with the air mass trajectory for each deposition. It became clear that: (a) The major component that acidifies atmospheric deposition is sulfuric acid. (b) Sulfate deposition increases in winter in the whole study area. (c) The sulfur isotopic ratios indicate that sulfur dioxide emitted from China affects the whole study area in winter. (d) Winter deposition of sulfate estimated to derive from coal combustion in China account for half of nss-sulfate deposition in average at 9 sites.