Specific Cleanup Research Articles

Antibody-mediated clean-up of blood for simultaneous HPLC determination of morphine and morphine glucuronides.

For the interpretation of the concentration of morphine in blood samples of heroin consumers information about the concentration of the analgesic active morphine metabolite morphine-6-glucuronide is very important. Thus a simple but specific clean-up procedure based on immuno-affinity chromatography is presented for the extraction of morphine, morphine-3-glucuronide and morphine-6-glucuronide from whole blood in cases of fatal heroin overdose. The preparation of the immunoabsorber by immobilization of antibodies against morphine-3-BSA and morphine-6-KLH with carbonyldiimidazole-activated trisacrylgel is described. The separation of the extracts is achieved by HPLC using native fluorescence detection. The limits of detection for this method are 10ng for morphine and morphine glucuronides/g blood. The results for the concentration of morphine and morphine glucuronides in blood from seven cases of heroin overdose are presented. By calculating the quotients for the concentrations of morphine-6-glucuronide/morphine the time elapsed since the last intake of heroin is estimated.

Optimization of monitoring well installation time and location during aquifer decontamination

An important question in the systematic and objective design of general-purpose ground-water quality monitoring networks is how to evaluate quantitatively the information they provide. However, many applications require the design of a groundwater monitoring network in conjunction with remedial action at a subsurface contamination site. In such a case, it is conceptually clear what is a successful network: One that reduces the net cost of meeting the objectives of cleanup. Uncertainty entails a cost because the natural management response to uncertainty is overdesign for the sake of conservatism (‘safety factor’). The additional information that the network provides must lead to cost reductions that outweigh its cost. This paper presents a method to determine the installation time and location of an additional monitoring well while the aquifer is being cleaned up. While rates of pumping and treatment are determined by the dual control method (a method for optimization with incomplete information) candidate well locations are ranked according to a ‘cost-to-go’ index that measures the costs expected until the goals of remediation are met. This index accounts for the cost associated with uncertainty about the system and thus is useful in appraising the value of information from new measurements in the context of the specific cleanup effort. The usefulness of the method is illustrated through application to a hypothetical two-dimensional aquifer with uncertain initial estimates of the system parameters and variables. Monte Carlo simulations demonstrate the cost effectiveness of solution obtained through this method.

A congener-specific method for the quantification of camphechlor (toxaphene) residues in fish and other foodstuffs

To develop a method for the quantification of camphechlor without the use of complex technical toxaphene as gas-chromatographic standard, all important chlorobornane peaks have been identified in a mixed marine fish sample reflecting the fish consumption in Germany. Further ECD but not ECNI-MS has been found to be suitable for estimation of the relative concentrations of chlorobornanes. The three camphechlor congeners with the highest ECD response have been found in concentrations of 0.05–0.08 mg/kg (fat basis), representing about 50% of the total chlorobornanes present. A predominance of these congeners has also been observed in a standard reference material of cod liver oil (SRM 1588). As these three congeners are presumed to be dominant in human camphechlor intake, it is proposed to use them as indicator components for a congener-specific analysis of camphechlor residues together with a fourth heptachlorobornane which does not accumulate in fish. Cleanup by gel permeation and silica gel chromatography with GC/ECD analysis has been tested for its suitability to determine these camphechlor congeners. The limit of determination found for each congener was about 5 μg/kg. The determination of these four congeners allows an unambiguous identification without specific cleanup (e.g. complete separation from PCBs or chlordanes) and a simple quantification of camphechlor residues, thus eliminating systematic errors resulting from different technical standards or detectors.

Determination of chloramphenicol in muscle, liver, kidney and urine of pigs by means of immunoaffinity chromatography and gas chromatography with electron-capture detection

A rapid and specific clean-up procedure based on immunoaffinity chromatography (IAC) with polyclonal antibodies for the gas chromatographic determination with electron-capture detection of chloramphenicol in pig muscle tissue, organs and urine is described. A commercially available IAC material was used for the analysis. A decrease in the capacity of the column after being used more than 100 times was observed. Mean recoveries were 69, 54, 62 and 95% for spiked pig muscle tissue, liver, kidney and urine, respectively. The limit of detection was 0.2 μg/kg for muscle tissue, 2.0 μg/kg for liver and kidney and 0.4 μg/kg for urine.

Recent advances in analytical methods for mycotoxins.

Recent advances in analytical methods are reviewed using the examples of aflatoxins and trichothecene mycotoxins. The most dramatic advances are seen as being those based on immunological principles utilized for aflatoxins to produce simple screening methods and for rapid specific clean-up. The possibilities of automation using immunoaffinity columns is described. In contrast for the trichothecenes immunological methods have not had the same general impact. Post-column derivatization using bromine or iodine to enhance fluorescence for HPLC detection of aflatoxins has become widely employed and there are similar possibilities for improved HPLC detection for trichothecenes using electrochemical or trichothecene-specific post-column reactions. There have been improvements in the use of more rapid and specific clean-up methods for trichothecenes, whilst HPLC and GC remain equally favoured for the end-determination. More sophisticated instrumental techniques such as mass spectrometry (LC/MS, MS/MS) and supercritical fluid chromatography (SFC/MS) have been demonstrated to have potential for application to mycotoxin analysis, but have not as yet made much general impact.

A Pipeline Spill into the Mersey Estuary, England

ABSTRACT On the 19th of August 1989 at 2:30 p.m., a fracture occurred in a pipeline carrying Venezuelan crude oil from a shipping terminal at Tranmere to the Shell (U.K.) Ltd. oil refinery at Stanlow, on the Mersey Estuary, England. 150 metric tons of oil were released into the estuary before the pipeline was sealed; tidal currents widely distributed the oil within a tidal cycle. The Mersey Estuary is heavily industrialized and urbanized but does retain extensive areas of salt marsh and intertidal mud flats which are internationally important for wildfowl and wading birds. Cleanup operations were coordinated by the two local fire brigades whose areas of responsibility included impacted shoreline. Input to the response came from government, local authorities, specialist consultants, and various other interested parties. The occurrence of the spill on one of the highest spring tides of the year and under favorable weather conditions served to lessen the environmental impacts. Less than two weeks after the spill, Shell (U.K.) and Cheshire County Council set up the Mersey Oil Spill Project Advisory Group, with a membership drawn from independent scientific groups, which would monitor the environmental effects of the spill and publish its findings. The primary report of the advisory group is a detailed historical record of the spill incident, the response to it, and the coordination of that response, as well as the lessons learned by the involved parties. Further studies consider the persistence of the oil, and its effects on birds, invertebrates, vegetation, and algae. Recommendations have already led to a review of the local contingency plan and the commissioning of work to produce specific cleanup guidelines and sensitivity maps for the region. In February 1990, a court action brought by the newly formed National Rivers Authority led to Shell (U.K.) Ltd. being fined £1 million due to the pollution arising from this incident.

Application of a 2,3,7,8-TCDD specific cleanup method for fish and sediments

Occidental Chemical Corporation participated in a study of Lake Ontario fish and sediments to quantitate levels of 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD). A 2,3,7,8-TCDD specific cleanup, developed at Occidental, was used to remove potentially interfering TCDD isomers as well as other interfering compounds. The extracts were then analyzed by GC/MS/MS. Sediments from Lake Ontario ranged in concentration from none detected at 1 pg/g to 360 pg/g. Fish samples ranged from none detected at 1 pg/g to 190 pg/g. Average surrogate recovery for sediments was 82% with a standard deviation of 13 and recovery for fish was 83% with a standard deviation of 15. In our experience this method, when compared to other 2,3,7,8-specific methods using carbon columns or HPLC to separate interferences, uses much less preparation time and is less prone to poor recoveries.

Determination of chloramphenicol in swine muscle tissue using a monoclonal antibody-mediated clean-up procedure

A rapid and specific clean-up procedure based on immunoaffinity chromatography for the high-performance liquid chromatographic determination of chloramphenicol (CAP) in swine muscle tissue at the 10 μg kg −1 level is described. For preparation of the columns, monoclonal antibodies against CAP were coupled to cyanogen bromide-activated Sepharose. After immunosorption of CAP from the aqueous meat extract, CAP was eluted with methanol. Mean recoveries from spiked swine muscle tissue were 70 ± 6% (10–50 μg kg −1 spiking levels). The loss of CAP can be completely attributed to the extraction; no loss was observed during the antibody-mediated clean-up.

Preliminary study of mycoflora and mycotoxins in grain dust from New Orleans area grain elevators.

Dust particles arising from disintegration of grain during handling and shipping may be inhaled by exposed barge and elevator workers. Since the normal grain mycoflora usually contain mycotoxin-producing fungi, these toxins could be natural contaminants of grain dust. Known mycoflora of commercial grain include species of Penicillium, Aspergillus, and Fusarium-fungi that may produce ochratoxins, aflatoxins and zearalenone. A procedure was developed to extract simultaneously these toxins from grain dust. Initial extraction with methylene chloride and water was followed by specific cleanup procedures for each toxin and then by thin layer chromatographic quantitation. In 50-g samples the lowest level of detection for zearalenone was 50 ng of zearalenone/g of dust, for ochratoxin, 10 ng/g and for aflatoxin, 5 ng/g. Dust samples were collected at various locations in two grain elevators and their associated transfer facilities in the New Orleans area. Large amounts of dust that had settled upon floors, machinery and ledges were tested, as well as that which had been collected by dust control systems. Samples were analyzed for aflatoxins, ochratoxin A, and zearalenone. None of the 15 samples contained any detectable amount of aflatoxins or ochratoxin A, but 10 of the 15 samples contained zearalenone at levels from 25 to 100 ng/g.

Preliminary Study of Mycoflora and Mycotoxins in Grain Dust from New Orleans Area Grain Elevators

Dust particles arising from disintegration of grain during handling and shipping may be inhaled by exposed barge and elevator workers. Since the normal grain mycoflora usually contain mycotoxin-producing fungi, these toxins could be natural contaminants of grain dust. Known mycoflora of commercial grain include species of Penicillium, Aspergillus, and Fusarium-fungi that may produce ochratoxins, aflatoxins and zearalenone. A procedure was developed to extract simultaneously these toxins from grain dust. Initial extraction with methylene chloride and water was followed by specific cleanup procedures for each toxin and then by thin layer chromatographic quantitation. In 50-g samples the lowest level of detection for zearalenone was 50 ng of zearalenone/g of dust, for ochratoxin, 10 ng/g and for aflatoxin, 5 ng/g. Dust samples were collected at various locations in two grain elevators and their associated transfer facilities in the New Orleans area. Large amounts of dust that had settled upon floors, machinery and ledges were tested, as well as that which had been collected by dust control systems. Samples were analyzed for aflatoxins, ochratoxin A, and zearalenone. None of the 15 samples contained any detectable amount of aflatoxins or ochratoxin A, but 10 of the 15 samples contained zearalenone at levels from 25 to 100 ng/g.

MARINE INDUSTRY GROUP (MIRG)

ABSTRACT Eleven companies involved in the marine transportation of petroleum in the Gulf of Mexico have established the Marine Industry Group (MIRG). MIRG is not an oil spill response organization, nor an oil spill cooperative. Rather, it is a group with the primary purpose of enhancing oil spill response capability in the Gulf of Mexico. Toward this end, MIRG has funded two oil spill contingency planning information projects which will:Identify the location of specific cleanup equipment and resources and provide information concerning the logistical requirements to deploy such equipmentProvide a survey which will identify and give information on the economically and ecologically sensitive areas in the Gulf of Mexico Both projects use available data and organize it into a format which can be useful for the broad area of interest where marine transporters operate. This paper describes the organization and objectives of MIRG, defines the area of interest, describes the resources and logistics and the environmental survey projects, and outlines other activities of the group. The resources and logistics project is discussed at length. The method of assembling the resource information, the verification process, and the updating methods are discussed. The use of this resource data is demonstrated for a hypothetical oil spill scenario.

Analysis of phenylethylamines in biological tissues by gas-liquid chromatography with electron-capture detection

2,4-Dinitrophenyl derivatives of phenylethylamines have been applied to the sensitive quantitative analysis of phenylethylamines in biological tissues by gas chromatography and electron-capture detection. The minimal detectable amounts are about 0.1 ng. A rapid and specific cleanup procedure allows the injection of 10% of all the amines extracted from 200 mg tissues, so that as little as 20 ng/gm tissue can be determined. Amines with or without hydroxyl groups can be determined as the DNP-derivatives with equal sensitivity. The corresponding 3,5-dinitro-4-trifluoromethyl derivatives were also prepared and their chromatographic behavior is reported.