Acaricide residues in beeswax. Implications in honey, brood and honeybee.

For beekeeping to be sustainable, the management of colonies for the production of bee products must be economically viable without endangering the lives of bees, and must include acceptable practices such as the treatment of hives with appropriate products. Occasionally, the use of acaricides to treat the hives against varroosis is uncontrolled and can accumulate in the hives, putting the colonies at risk. In this work, a screening of seven acaricides was carried out in different apiaries in Andalusia (Spain). Their distribution in beeswax, brood, honey, and bees from colonies in different surroundings was evaluated at different times. It was found that beeswax was highly contaminated but honey, brood and bees had acceptable levels, below their respective MRL or LD50, after a certain period following varrocide treatments. Acaricides banned for their use against Varroa, such as chlorfenvinphos, cypermethrin and especially acrinathrin, were found in the hives analysed.

Determination of Regulated and Emerging Mycotoxins in Organic and Conventional Gluten-Free Flours by LC-MS/MS.

Gluten-free cereal products have grown in popularity in recent years as they are perceived as "healthier" alternatives and can be safely consumed by celiac patients, and people with gluten intolerance or wheat allergies. Molds that produce mycotoxins contaminate cereal crops, posing a threat to global food security. Maximum levels have been set for certain mycotoxins in cereal flours; however, little is known about the levels of emerging mycotoxins in these flours. The aim of this study was to develop an efficient, sensitive, and selective method for the detection of four emerging (beauvericin and enniatins A1, B, and B1) and three regulated (aflatoxin B1, zearalenone, and deoxynivalenol) mycotoxins in gluten-free flours. Ultrasound-assisted matrix solid-phase dispersion was used in the extraction of these mycotoxins from flour samples. The validated method was utilized for the LC-MS/MS analysis of conventional and organic wholegrain oat and rice flours. Six of the seven target mycotoxins were detected in these samples. Multi-mycotoxin contamination was found in all flour types, particularly in conventional wholegrain oat flour. Despite the low detection frequency in rice flour, one sample was found to contain zearalenone at a concentration of 83.2 µg/kg, which was higher than the level set by the European Commission for cereal flours. The emerging mycotoxins had the highest detection frequencies; enniatin B was present in 53% of the samples at a maximum concentration of 56 µg/kg, followed by enniatin B1 and beauvericin, which were detected in 46% of the samples, and at levels reaching 21 µg/kg and 10 µg/kg, respectively. These results highlight the need to improve the current knowledge and regulations on the presence of mycotoxins, particularly emerging ones, in gluten-free flours and cereal-based products.

Simultaneous Determination of 15 Mycotoxins in Aquaculture Feed by Liquid Chromatography-Tandem Mass Spectrometry.

The use of plant-based fish feed may increase the risk of contamination by mycotoxins. The multiresidue analysis of mycotoxins in fish feed presents many difficulties due to the complexity of the matrix, the different characteristics of the compounds, and their presence in highly different concentration levels. The aim of this study was to develop a selective, sensitive, and efficient analytical method for the simultaneous determination of 15 mycotoxins (regulated and emerging mycotoxins) in aquaculture feed by LC-MS/MS. Sample extraction was performed with ultrasonic assistance, and different cleanup strategies were evaluated. The optimized method was composed by ultrasound-assisted extraction (two cycles, 55 °C, 20 min), followed by cleanup using a Captiva EMR Lipid cartridge. Then, nine commercial samples of aquaculture fish feed were analyzed. Eight of the 15 target mycotoxins were detected in the samples. Results showed that two enniatins (EENB and ENNB1), beauvericin, and fumonisin B2 were detected in all samples. These results show the multi-mycotoxin contamination of fish feed, highlighting the need to improve current knowledge on the occurrence and toxicity of mycotoxins in fish feed, mainly the emerging ones.

Determination of Emerging Contaminants in Cereals by Gas Chromatography-Tandem Mass Spectrometry.

Cereals are staple foods for human consumption in both developed and developing countries. In order to improve agricultural outputs, resources like reclaimed water for irrigation and biosolids and manure as fertilizers are frequently used, although they may increase the input of contaminants that can potentially be absorbed by crops and enter the food chain. Emerging contaminants (human and veterinary pharmaceuticals, personal care products, surfactants, plasticizers, and industrial additives, among others) are continuously introduced in the environment from a variety sources and these contaminants may enter the food chain through plant uptake. In this study, an analytical method, based on ultrasound-assisted extraction and dispersive solid-phase cleanup, was developed for the determination of emerging contaminants from different classes in four highly consumed cereal grains (wheat, oat, barley, and rice). These analytes were selected considering the results of our previous studies carried out in soil and vegetables and those frequently detected in real samples were chosen. The target compounds selected were bisphenol A (BPA), bisphenol F (BPF), methyl paraben, propyl paraben, linear chain nonylphenol in position 4 (4-n-NP), mixture of ring and chain isomers of NP and six pharmaceutical compounds (allopurinol, mefenamic acid, carbamazepine, paracetamol, diclofenac and ibuprofen). Recoveries ranging from 68 to 119% with relative standard deviations (RSD) <18% were obtained for all the compounds except for allopurinol, with recoveries that ranged from 30 to 66% with RSD ≤ 12% and the limits of detection achieved ranged from 0.03 to 4.9 ng/g. The method was applied to the analysis of 16 cereal samples, ten were purchased in local supermarkets and the rest were collected directly from agricultural fields, five of which were fertilized with organic amendments. Bisphenol A (BPA) was detected in all samples at levels that ranged from 1.6 to 1,742 ng/g. Bisphenol F, a substitute for BPA, was also found in six samples (up to 22 ng/g). Linear 4-n-NP was found in a reduced number of samples but the mixture of NP isomers was found in all the samples, being the mean concentrations in wheat, barley, oat and rice 49, 90, 142, and 184 ng/g, respectively.

Assessing the benefits of composting poultry manure in reducing antimicrobial residues, pathogenic bacteria, and antimicrobial resistance genes: a field-scale study.

The poultry industry in the European Union produces 13 million tons of manure annually, which represents a major health and environmental challenge. Composting is an environmental-friendly technique for the management of manure, but there are few studies about antibiotic residues and antimicrobial resistances at a field scale. The goal of this study was to determine if the composting of poultry manure at a field scale would result in the reduction of antibiotic residues, pathogenic bacteria, and antibiotic resistance genes (ARGs) in the final fertilizer product. A 10-week composting of poultry manure spiked with enrofloxacin, doxycycline, and ciprofloxacin was performed. The determination of antibiotics residues and 22 selected ARGs was carried out together with the identification of bacteria by metagenomics. In the case of ciprofloxacin and doxycycline, a 90% decrease was observed after composting for 3 weeks. Sixteen ARGs were detected at the beginning of the experiment; 12 of them decreased from week 0 to week 10 (reduction of 73.7-99.99%). The presence of potentially pathogenic bacteria, such as, Campylobacter coli or commensal bacteria such as Escherichia coli decreases along the composting process. In conclusion, 10-week composting of poultry manure promotes the reduction of antibiotic residues and most of the ARGs and pathogenic bacteria.

Analysis of Multiclass Antibiotics in Lettuce by Liquid Chromatography-Tandem Mass Spectrometry to Monitor Their Plant Uptake.

The main entry routes of antibiotics in the environment are the application of organic wastes to improve soil quality and the irrigation with recycled water. Once in the environment, antibiotics can be introduced in the food chain through their uptake by crops. This paper describes the development of an analytical method based on ultrasound-assisted extraction for the determination of seven antibiotics in lettuce. The developed method was applied to evaluate antibiotic uptake by lettuce grown in pots fertilized with composted poultry litter doped with a mixture of antibiotics to reach a final concentration of 2.5 µg/g in soil. Lettuce were harvested after 21, 36, and 55 days. Five of the seven studied antibiotics were found in all samples. The highest uptake was found for lincomycin (51 ng/g fresh weight) followed by sulfamethoxazole (44 ng/g fresh weight) and sulfamethazine (21 ng/g fresh weight) in lettuce harvested after 21 days. An important decrease of their levels was observed after 36 days, but these levels remained similar after 55 days. Although levels found in lettuce were low, the presence of antibiotics demonstrates the need for further assessing food safety risks related with the use of soil amendments or irrigation water contaminated with antibiotics.

Rapid determination of antibiotic residues in cereals by liquid chromatography triple mass spectrometry.

Antibiotics may be present in agricultural soils through the application of organic amendments as fertilizers or by irrigation of fields with recycled water. As a result of these agricultural practices, antibiotics in soil can lead to their uptake by plants, entering in this way the food chain. Studies on the levels of antibiotics in cereal samples are scarce in the available literature. In this work, an analytical method was developed for the determination of 19 antibiotics (fluoroquinolones, sulfonamides, tetracyclines, and lincosamides) in four types of cereal grains (wheat, barley, rice, and oat). Ultrasound-assisted matrix solid-phase dispersion was selected as extraction technique with recoveries of target analytes ranging from 73 to 127% for the four cereals analyzed. Limits of quantification obtained ranged from 0.8 to 5.8 ng g-1. Compared with methods described for the analysis of antibiotics in cereals, the developed method uses a lower volume of extraction solvent and very good recoveries were obtained for all compounds. The validated method was applied to the analysis of different types of cereals samples, harvested from agricultural fields or purchased from local supermarkets. The analysis of the five cereal samples grown in fields with 3 years of consecutive organic amendments revealed that none of the nineteen antibiotics selected were found in any sample. Eleven commercial samples of cereals of different types and presentations were analyzed and enrofloxacin was detected in one rice sample; the presence of enrofloxacin in cereals or its incorporation into crops from soil or water not previously reported. Graphical abstract.

Molecularly imprinted polymer-hollow fiber microextraction of hydrophilic fluoroquinolone antibiotics in environmental waters and urine samples.

In the present work, the preparation of a new selective molecularly imprinted polymer (MIP) for the family of fluoroquinolones (FQs) in the pores of polypropylene hollow fibers (HFs) is proposed. The resulting MIP-HFs, which combine solid-phase microextraction (SPME) and molecular imprinting technologies, were used to develop a selective microextraction methodology (MIP-HFM) to determine selected FQs danofloxacin, norfloxacin, enrofloxacin and ciprofloxacin in real samples of environmental and biological interest. Measurements during the optimization of the MIP-HFM and its application to the analyses of real samples were performed by HPLC-UV and HPLC-MS/MS. In order to establish optimum rebinding conditions, the effect of key experimental parameters such as loading media, extraction time and stirring-rate were studied. The developed MIP composites exhibited recognition properties towards the selected hydrophilic antibiotics in non-polar media (toluene) and in polar protic systems such as methanol and methanol/water solutions, up to 20% water content. Recoveries by the developed method for all FQs tested in surface water, groundwater and urine spiked with the analytes of interest at two different concentration levels were within 9.4-24.5 %, with a relative standard deviation, generally <20% (n = 3). The detection limits were within 0.1-10 µg L-1, depending upon the antibiotic and the type of sample.

Persistence and availability of veterinary antibiotics in soil and soil-manure systems.

The availability and persistence of various antibiotics in soil and soil amended with composted poultry manure were investigated through laboratory incubation assays. Six veterinary antibiotics (one fluoroquinolone, two tetracyclines, two sulfonamides and one lincosamide) and one active metabolite (ciprofloxacin) were studied. The incubation assays were conducted at a controlled temperature of 25 °C with different water regimes, such as constant moisture content (80% of water holding capacity) and drying-rewetting cycles. The studied antibiotics were determined in soil and soil aqueous phase samples by LC-MS/MS using internal standards. The results indicated that the highest levels found in the soil aqueous phase were for sulfamethoxazole, followed by sulfamethazine and lincomycin, being very low the levels of chlortetracycline, doxycycline, ciprofloxacin and enrofloxacin (≤1.8%). A positive correlation was observed between the antibiotic concentrations and the content of the dissolved organic carbon in soil aqueous phase with the incubation time. An increase in the apparent sorption coefficients of these antibiotics, except chlortetracycline and lincomycin, was observed when the soil was amended with composted manure. Except for fluoroquinolones, with remaining residues around 70% after 90 days of incubation, a fast dissipation of antibiotics was observed during the assay, with half-lives ranging from 8 to 27 days. These values increased between 6% and 53% in manure amended soil; nevertheless, half-lives remained short (9 days and 27 days for lincomycin and sulfamethazine, respectively). Similar results were obtained with soil under drying-rewetting cycles showing somewhat lower values in soil aqueous phase and slightly shorter half-lives in some cases. The results obtained pointed out that the route of entry of antibiotics into the soil, through recycled water or manure, may have an important effect on their behavior, particularly regarding their availability in soil.

Analysis of emerging organic contaminants in poultry manure by gas chromatography-tandem mass spectrometry.

A multiresidue method was developed for the determination of 19 emerging organic contaminants (pharmaceutical drugs, personal care products, and bisphenol A) in poultry manure. Lyophilized samples of manure were extracted by ultrasound-assisted matrix solid-phase dispersion and the extracts were analyzed by gas chromatography with tandem mass spectrometry after derivatization. Analysis of spiked poultry manure samples, at levels ranging from 25 to 150 ng/g, gave satisfactory recovery results for all the compounds, with values from 67 to 106%. The developed procedure provided detection limits that ranged from 0.9 to 2.2 ng/g. Finally, the validated method was applied to poultry manure samples collected from 23 poultry farms in Spain. Salicylic acid was found in most of the samples analyzed at levels up to 2501 ng/g, whereas, methyl paraben, orthophenylphenol, ibuprofen, paracetamol, and carbamazepine were detected at levels up to 250 ng/g. Composting of manure showed an important decrease in the levels of the detected contaminants.

Analysis of macrolide antibiotics in water by magnetic solid-phase extraction and liquid chromatography-tandem mass spectrometry.

Macrolides are one of the most commonly used families of antibiotics employed in human and veterinary treatment. These compounds are considered emerging contaminants with potential ecological and human health risks that could be present in surface water. This paper describes the development and application of a simple and efficient extraction procedure for the determination of tilmicosin; erythromycin, tylosin and erythromycin-H2O from water samples. Sample extraction was carried out using magnetic solid-phase extraction using oleate functionalized magnetic nanoparticles followed by LC-MS/MS analysis. The effects of several parameters on the extraction efficiency of MLs from water were evaluated. The recovery results obtained were >84% for most of the compounds, except for erytromycin. The LOD and LOQ values ranged from 11.5 to 26ngL-1 and from 34 to 77ngL-1, respectively. The selected method was applied to monitor these contaminants in water samples from different sources. Tilmicosin and tylosin were not detected in any of the samples, but erythromycin and erythromycin-H2O were found in 50% of the surface water samples at levels from

Rapid multiresidue determination of bisphenol analogues in soil with on-line derivatization.

Bisphenol analogues are compounds extensively used which have been potentially linked to adverse health effects. Nevertheless, few studies reported the analysis of compounds, other than bisphenol A, in environmental solid samples and none in soil samples. In this study, a rapid and sensitive analytical method is presented for the simultaneous determination of 13 bisphenols in soil samples. The method combines ultrasonic-assisted extraction of samples placed in small columns and GC-MS/MS analysis. Manual and on-line derivatizations were compared and results showed that significant higher chromatographic responses were achieved with on-line derivatization. Different parameters such as the quantity of derivatization agent, the extraction solvent, or the extraction time were assayed. The detection limits for all target bisphenols ranged from 0.04 to 0.27 ng g-1, for BPC and BPA, respectively. Analysis of spiked soil samples gave satisfactory recovery results, from 70 to 111%, for all the compounds. Finally, the validated method was applied to soil samples from several Spanish areas, and 3 of the 13 target bisphenols (BPAF, BPF, and BPA) were detected, although only BPF and BPA could be quantified with levels up to 127 ng g-1. Graphical abstract Schematic diagram of the developed method for the determination of bisphenol analogues.

Simultaneous determination of multiclass emerging contaminants in aquatic plants by ultrasound-assisted matrix solid-phase dispersion and GC-MS.

A multiresidue method was developed for the simultaneous determination of 31 emerging contaminants (pharmaceutical compounds, hormones, personal care products, biocides, and flame retardants) in aquatic plants. Analytes were extracted by ultrasound-assisted matrix solid-phase dispersion (UA-MSPD) and determined by gas chromatography-mass spectrometry after sylilation, The method was validated for different aquatic plants (Typha angustifolia, Arundo donax, and Lemna minor) and a semiaquatic cultivated plant (Oryza sativa) with good recoveries at concentrations of 100 and 25 ng g-1 wet weight, ranging from 70 to 120 %, and low method detection limits (0.3 to 2.2 ng g-1 wet weight). A significant difference of the chromatographic response was observed for some compounds in neat solvent versus matrix extracts, and therefore, quantification was carried out using matrix-matched standards in order to overcome this matrix effect. Aquatic plants taken from rivers located at three Spanish regions were analyzed, and the compounds detected were parabens, bisphenol A, benzophenone-3, cyfluthrin, and cypermethrin. The levels found ranged from 6 to 25 ng g-1 wet weight except for cypermethrin that was detected at 235 ng g-1 wet weight in O. sativa samples.

Application of matrix solid-phase dispersion followed by GC-MS/MS to the analysis of emerging contaminants in vegetables.

A multiresidue method for the determination of 17 emerging contaminants in vegetables was developed based on ultrasound-assisted matrix solid-phase dispersion (MSPD). The analysis was performed using isotope dilution gas chromatography tandem mass spectrometry. In the development of the MSPD procedure, different parameters such as sonication and the type of sorbent or extraction solvent were assayed. Manual and in situ derivatization was assayed and the chromatographic response was higher when the reaction takes place in the injection port. The limits of detection obtained for the studied compounds were in the range of 0.1-0.4ngg(-1) for the different vegetables analyzed. The developed method was applied to vegetables obtained from several local markets. At least one of the organophosphates was detected in the analyzed samples at levels ranging from 0.6 to 4.6ngg(-1) and bisphenol A was detected in all the samples at concentration up to 16ngg(-1).

Determination of endocrine-disrupting compounds in water samples by magnetic nanoparticle-assisted dispersive liquid-liquid microextraction combined with gas chromatography-tandem mass spectrometry.

A rapid extraction procedure is presented for the determination of five endocrine-disrupting compounds, estrone, ethinylestradiol, bisphenol A, triclosan, and 2-ethylhexylsalicylate, in water samples. The analysis involves a two-step extraction procedure that combines dispersive liquid-liquid microextraction (DLLME) with dispersive micro-solid phase extraction (D-µ-SPE), using magnetic nanoparticles, followed by in situ derivatization in the injection port of a gas chromatograph coupled to triple quadrupole mass spectrometry. The use of uncoated or oleate-coated Fe3O4 nanoparticles as sorbent in the extraction process was evaluated and compared. The main parameters involved in the extraction process were optimized applying experimental designs. Uncoated Fe3O4 nanoparticles were selected in order to simplify and make more cost-effective the procedure. DLLME was carried out at pH 3, during 2 min, followed by the addition of the nanoparticles for D-µ-SPE employing 1 min in the extraction. Analysis of spiked water samples of different sources gave satisfactory recovery results for all the compounds with detection limits ranging from 7 to 180 ng l-1. Finally, the procedure was applied in tap, well, and river water. Graphical abstract Diagram of the extraction method using magnetic nanoparticles (MNPs).

Application of magnetic iron oxide nanoparticles for the analysis of PCBs in water and soil leachates by gas chromatography-tandem mass spectrometry.

Two magnetic solid-phase extraction methods (mSPE) were developed and compared for the extraction and preconcentration of polychlorinated biphenyls (PCBs) from water and soil leachates. Analyses were carried out by gas chromatography coupled to triple quadrupole mass spectrometry. The mSPE extraction parameters were optimised using Fe3O4 nanoparticles coated with palmitate or oleate. Differences were found between the developed mSPE methods depending on the magnetic nanoparticle coating. The extraction efficiency of both sorbents was studied by spiking soil leachates at three concentration levels (from 0.6 to 0.18 ng ml(-1) and from 0.4 to 0.04 ng ml(-1) using palmitate or oleate coated nanoparticles, respectively) and recoveries from 86 to 109 % were obtained. The developed method provided a preconcentration factor of 250. The detection limits were about 29 times lower with the oleate-coated nanoparticles. Although both mSPE procedures could be used for the extraction of PCBs from water and soil leachates, oleate-coated nanoparticles gave the best extractive conditions and lower quantifications limits. Finally, the mSPE using oleate-coated nanoparticles was applied to the analysis of PCBs in river waters and in soil leachates obtained from soil with different physico-chemical characteristics. The levels of PCBs present in the leachates depended on the soil sample. The present work demonstrates the applicability of both mSPE methods to the determination of PCBs in water and soil leachates, which is of interest for mobility and bioavailability studies of these compounds in soil.

Multiresidue analysis of insecticides and other selected environmental contaminants in poultry manure by gas chromatography/mass spectrometry.

An analytical method was developed for the simultaneous determination in poultry manure of 41 organic contaminants belonging to different chemical classes: pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls, and polybrominated diphenyl ethers. Poultry manure was extracted with a modified QuEChERS method, and the extracts were analyzed by isotope dilution GC/MS. Recovery of these contaminants from samples spiked at levels ranging from 25 to 100 ng/g was satisfactory for all the compounds. The developed procedure provided LODs from 0.8 to 9.6 ng/g. The analysis of poultry manure samples collected on different farms confirmed the presence of some of the studied contaminants. Pyrethroids and polycyclic aromatic hydrocarbons were the main contaminants detected. DDT and its metabolite DDE were also found but at relatively low concentrations.

Rapid determination of natural and synthetic hormones in biosolids and poultry manure by isotope dilution GC-MS/MS.

The release of hormones into the environment due to land application of biosolids and manure is a cause of concern for their potential impacts. This paper presents the development of a rapid and sensitive method, based on extraction, for the analysis of 13 hormones in biosolids and poultry manure. A simultaneous derivatization of hydroxyl and ketone groups was carried out for the determination of hormones by GC­MS/MS. The method was validated in three matrices (sewage sludge, manure, and broiler litter). Recoveries from spiked samples at three concentration levels (50, 25, and 10 ng/g) ranged from 76 to 124% with relative SDs ≤ 16%. Method detection limits for the three matrices were in the range of 0.5­3.0 ng/g dry weight. The optimized method was applied to biosolid and poultry manure samples collected in Spain. Only seven of the 13 studied hormones were detected in the different samples. trans-Androsterone was detected at high levels (up to 3.1 µg/g in biosolid samples). Estrone and estradiol were the two hormones detected at higher levels in layer manure, whereas estrone and 4-androstene-3,17-dione presented the highest levels in broiler litter.

Determination of selected pharmaceutical compounds in biosolids by supported liquid extraction and gas chromatography-tandem mass spectrometry.

In this work, an analytical method was developed for the determination of pharmaceutical drugs in biosolids. Samples were extracted with an acidic mixture of water and acetone (1:2, v/v) and supported liquid extraction was used for the clean-up of extracts, eluting with ethyl acetate:methanol (90:10, v/v). The compounds were determined by gas chromatography-tandem mass spectrometry using matrix-match calibration after silylation to form their t-butyldimethylsilyl derivatives. This method presents various advantages, such as a fairly simple operation for the analysis of complex matrices, the use of inexpensive glassware and low solvent volumes. Satisfactory mean recoveries were obtained with the developed method ranging from 70 to 120% with relative standard deviations (RSDs) ≤ 13%, and limits of detection between 0.5 and 3.6 ng g(-1). The method was then successfully applied to biosolids samples collected in Madrid and Catalonia (Spain). Eleven of the sixteen target compounds were detected in the studied samples, at levels up to 1.1 µg g(-1) (salicylic acid). Ibuprofen, caffeine, paracetamol and fenofibrate were detected in all of the samples analyzed.

Occurrence and analysis of selected pharmaceutical compounds in soil from Spanish agricultural fields.

This work describes the analysis of 15 pharmaceutical compounds, belonging to different therapeutic classes (anti-inflammatory/analgesics, lipid regulators, antiepileptics, ß-blockers and antidepressants) and with diverse physical-chemical properties, in Spanish soils with different farmland uses. The studied compounds were extracted from soil by ultrasound-assisted extraction (UAE) and determined, after derivatization, by gas chromatography with mass spectrometric detection (GC-MS). The limits of detection (LODs) ranged from 0.14 ng g(-1) (naproxen) to 0.65 ng g(-1) (amitriptyline). At least two compounds where detected in all samples, being ibuprofen, salicylic acid, and paracetamol, the most frequently detected compounds. The highest levels found in soil were 47 ng g(-1) for allopurinol and 37 ng g(-1) for salicylic acid. The influence of the type of crop and the sampling area on the levels of pharmaceuticals in soil, as well as their relationship with soil physical-chemical properties, was studied. The frequent and widespread detection of some of these compounds in agricultural soils show a diffuse contamination, although the low levels found do not pose a risk to the environment or the human health.