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Background: In field experiments, assessment of herbicide selectivity and efficacy rarely takes advantage of dose-response regressions. The objective is to demonstrate that logarithmic sprayers, which automatically make a logarithmic dilution of a herbicide rate, can extract biologically relevant parameters describing the efficacy of herbicides in crops, and compare localities and time of assessment., Results: In a conventional and an organic field, canola, white mustard, and no crop plots were sprayed with diflufenican and beflubutamid. A mixed effect log-logistic dose-response regression, with autoregressive correlation structure, estimated ED 50 and ED 90 for visual and Excess Green Index symptoms at various days after treatment (DAT). For visual assessment, ED 50 differed within no crop between locations for beflubutamid at 12 DAT and 26 DAT. For diflufenican, the ED 50 was different within crops at the two fields at 12 DAT, but not at 26 DAT. The Excess Green Indices at ED 50 were not different among herbicides, locations, and corps; ED 90 differed for white mustard and canola for beflubutamid but not for diflufenican., Conclusion: Suitable nonlinear regression models are now available for fitting dose-response data from a logarithmic sprayer in field experiments. The derived parameters (e.g. ED 50 ) can compare selectivity and efficacy at numerous cropping systems. © 2018 Society of Chemical Industry., (© 2018 Society of Chemical Industry.)

Background: Bifora radians, an annual weed in winter wheat, is distributed mainly in the Mediterranean area, Asia Minor and the Caucasus. It infests winter-sown crops of the Central Anatolia and Middle Black Sea regions of Turkey. Field experiments in heavily B. radians-infested fields were conducted over 3 years in Samsun, Turkey, to determine the response of B. radians to ALS-inhibiting herbicides, because growers had complained of a decrease in herbicide effect., Results: The efficacy of ALS inhibitors on a putatively tolerant population sprayed annually with ALS inhibitors and an adjacent allegedly sensitive population was estimated at the ED(50) and ED(90) response levels. The recommended rates of herbicides controlled 90% of the weed (ED(90)) in the sensitive population at the early stage of B. radians development, but not in the tolerant population. The relative potencies (ED(x(tolerant))/ED(x(sensitive))) of herbicides on the two populations were estimated by assuming years as being random effects. The relative potency was on average about 1.7, irrespective of the ED(x) levels., Conclusion: Although the relative potencies were not large, they were large enough to be noted by growers. In field experiments it would be important to establish tools demonstrating when farmers recognise loss of herbicide efficacy. There has been no indication of evolution of resistant biotypes so far, but continuous spraying favours biotypes with increased levels of tolerance., (Copyright © 2011 Society of Chemical Industry.)

Background: Grass seed crops are minor crops that cannot support the development of selective herbicides for grass weed control in grass seed crops. An option is to screen for selective herbicides with the use of logarithmic spraying technology. The aim of this paper is to assess selectivity of various herbicides in grass seed crops by using dose-response curves., Results: Six grass species were subjected to logarithmic spraying with 11 herbicides and with Poa pratensis L. as a weed. The ratio between the doses that caused 10% of damage to the crop and 90% of damage to the weed was used as a selectivity index. Compounds with selectivity indices above 2 can be safely used in a crop. The two ACCase herbicides clodinafop-propargyl and fenoxaprop-P-ethyl and a mixture of the two ALS herbicides mesosulfuron and iodosulfuron could be used selectively to control P. pratensis in Festuca rubra L., although the selectivity indices in no instances were greater than the desired 2.0., Conclusion: The logarithmic sprayer can be a rapid screening tool for identifying compounds with favourable selectivity indices. Good experimental design is needed to alleviate rates being systematically distributed and confounded with growth rate and soil fertility gradients., ((c) 2009 Society of Chemical Industry.)

For plants, pigment content has shown to be a remarkably consistent biomarker across chemicals with different modes of action. In this study, we evaluated the use of pigment content as endpoint in binary mixture toxicity studies compared to three growth endpoints on the floating plant Lemna minor. Six binary combinations of six herbicides with different mode of action were used. Data were tested against both the concentration addition (CA) and independent action (IA) reference models. For CA, two statistical approaches were used. The study showed that for some herbicide combinations the mixture toxicity measured on pigment content did not reflect the results measured on plant population growth, emphasizing the importance of measuring growth in parallel with biomarkers. CA explained the data just as well as IA, and the two different statistical models used to test the data in relation to CA showed very similar results.

Desmedipham, phenmedipham and a 50% mixture of the two decreased the maximum quantum efficiency of photosystem II (F(v)/F(m)) and the relative changes at the J step (F(vj)) immediately after spraying in both sugar beet and black nightshade grown in the greenhouse. Sugar beet recovered more rapidly from phenmedipham and the mixture than from desmedipham. Desmedipham and the mixture irreversibly affected F(v)/F(m) and F(vj) in black nightshade at much lower doses than in sugar beet. Black nightshade recovered from phenmedipham injury at the highest dose in the first experiment (120 g AI ha(-1)) but not in the second experiment (500 g AI ha(-1)). The dry matter dose-response relationships and the energy pipeline presentation confirmed the same trend. There was a relatively good correlation between F(vj) taken 1 day after spraying and dry matter taken 2 or 3 weeks after spraying. The differential speed of herbicide metabolism between weed and crop plays an important role in herbicide selectivity and can be studied by using appropriate chlorophyll a fluorescence parameters., (Copyright 2007 Society of Chemical Industry.)

Risk assessment of herbicides towards non-target plants in Europe is currently based solely on tests on algae and floating aquatic plants of Lemna sp. Effects on terrestrial non-target species is not systematically addressed. The purpose of the present study was to compare combination effects of herbicide mixtures across aquatic and terrestrial test systems, and to test whether results obtained in the traditional aquatic test systems can be extrapolated to the terrestrial environment. This was done by evaluating ten binary mixtures of nine herbicides representing the seven most commonly used molecular target sites for controlling broadleaved weeds. Data were evaluated statistically in relation to the concentration addition model, and for selected concentrations to the independent action model. The mixtures were tested on the terrestrial species Tripleurospermum inodorum (L.) Schultz-Bip. (Scentless Mayweed) and Stellaria media (L.) Vill. (Common Chickweed), and on the aquatic species Lemna minor L. (Lesser duckweed) and the alga Pseudokirchneriella subcapitata (Korschikov) Hindak. For the two mixtures of herbicides with the same molecular site of action, the joint effect was additive. For the eight mixtures of herbicides with different sites of action, two of the mixtures were consistently antagonistic across species, while for the remaining six mixtures the joint effect depended on the species tested. This dependence was, however, not systematic, in the sense that none of the species or test systems (terrestrial versus aquatic) had a significantly higher probability of showing synergistic or antagonistic joint effects than others. Synergistic interactions were not observed, but approximately 70% of the mixtures of herbicides with different sites of action showed significant antagonism. Hence, the concentration addition model can be used to estimate worst-case effects of mixtures of herbicides on both terrestrial and aquatic species. Comparing the sensitivity of the species to a 10% spray drift event showed that the terrestrial species were more vulnerable to all herbicides compared with the aquatic species, emphasising the importance of including terrestrial non-target plants in herbicide risk assessment., (Copyright 2007 Society of Chemical Industry.)

The joint action of soil-applied herbicide mixtures with similar or different modes of action has been assessed by using the additive dose model (ADM). The herbicides chlorsulfuron, metsulfuron-methyl, pendimethalin and pretilachlor, applied either singly or in binary mixtures, were used on rice (Oryza sativa L.). The growth (shoot) response curves were described by a logistic dose-response model. The ED50 values and their corresponding standard errors obtained from the response curves were used to test statistically if the shape of the isoboles differed from the reference model (ADM). Results showed that mixtures of herbicides with similar molecular targets, i.e. chlorsulfuron and metsulfuron (acetolactate synthase (ALS) inhibitors), and with different molecular targets, i.e. pendimethalin (microtubule assembly inhibitor) and pretilachlor (very long chain fatty acids (VLCFAs) inhibitor), followed the ADM. Mixing herbicides with different molecular targets gave different results depending on whether pretilachlor or pendimethalin was involved. In general, mixtures of pretilachlor and sulfonylureas showed synergistic interactions, whereas mixtures of pendimethalin and sulfonylureas exhibited either antagonistic or additive activities. Hence, there is a large potential for both increasing the specificity of herbicides by using mixtures and lowering the total dose for weed control, while at the same time delaying the development of herbicide resistance by using mixtures with different molecular targets., (Copyright (c) 2006 Society of Chemical Industry.)

During the past two decades, the phenomenon of hormesis has gained increased recognition. To promote research in hormesis, a sound statistical quantification of important parameters, such as the level and significance of the increase in response and the range of concentration where it occurs, is strongly needed. Here, we present an improved statistical model to describe hormetic dose-response curves and test for the presence of hormesis. Using the delta method and freely available software, any percentage effect dose or concentration can be derived with its associated standard errors. Likewise, the maximal response can be extracted and the growth stimulation calculated. The new model was tested on macrophyte data from multiple-species experiments and on laboratory data of Lemna minor. For the 51 curves tested, significant hormesis was detected in 18 curves, and for another 17 curves, the hormesis model described that data better than the logistic model did. The increase in response ranged from 5 to 109%. The growth stimulation occurred at an average dose somewhere between zero and concentrations corresponding to approximately 20 to 25% of the median effective concentration (EC50). Testing the same data with the hormesis model proposed by Brain and Cousens in 1989, we found no significant hormesis. Consequently, the new model is shown to be far more robust than previous models, both in terms of variation in data and in terms of describing hormetic effects ranging from small effects of a 10% increase in response up to effects of an almost 100% increase in response.

Widely used herbicides sometimes inadvertently contaminate surface waters. In this study we evaluate the toxicity of herbicides to aquatic plants and algae and relate it to environmental herbicide concentrations and exposure scenarios, herbicide formulation and mode of action. This was done experimentally for ten herbicides, using the aquatic macrophyte Lemna minor L. and the green alga Pseudokirchneriella subcapitata (Korshikov) Hindak, supplemented with a database study comprising algae toxicity data for 146 herbicides. The laboratory study showed that herbicide formulations in general did not enhance herbicide efficacy in the aquatic environment. The Roundup formulation of glyphosate proved to be the only exception, decreasing the EC(50) of the technical product for both L. minor and P. subcapitata approximately fourfold. Comparison of the sensitivity of L. minor and P. subcapitata revealed up to 1000-fold higher sensitivity of L. minor for the herbicides categorized as weak acids (pK(a) < 5), emphasizing the importance of higher plants in hazard assessment. Database analyses showed that no herbicide group, categorized by site of action, was significantly more toxic than another. Synthetic auxins were the exception as they are virtually non-toxic to unicellular algae. There was no strong correlation between toxicity to algae and K(ow) of the herbicides, not even within groups having the same site of action. Evaluating all data, few herbicides were toxic at concentrations below 1 microg l(-1), which is the 99.9th percentile of the herbicide concentrations measured in the Danish surveillance programme. Joint action of several herbicides cannot however be excluded.

Theoretically, the effect of two independently acting compounds in a mixture will depend on the slope of the dose-response curves of the individual compounds if evaluated in relation to the model of concentration addition (CA). In the present study, we explored development of the shape of the dose-response relationship for four different recommended endpoints (surface area, frond number, fresh weight-specific, and dry weight-specific relative growth rates [RGRA, RGRF, RGRFW, and RGRDW, respectively]) and for two differently acting herbicides (metsulfuron-methyl and terbuthylazine) over time (3-15 d) on the standard test plant Lemna minor to identify endpoints and experiment times for which predictions of independent action (IA) would depart the most from those of CA. After a test time of 6 d, predictions of IA based on RGRA and RGRFW showed antagonism in relation to CA. Based on RGRDW, synergy was predicted, whereas IA based on RGRF was indistinguishable from CA. To test the prediction of choice of endpoint giving different results in mixture-toxicity experiments, three endpoints and six combinations of independently acting herbicides were evaluated using isobolograms. The experiments showed that in four of six herbicide combinations, different conclusions were reached depending on endpoint. The contradictory isoboles did not follow the theory of IA and, therefore, are more likely to be related to differences in susceptibility of the physiological processes affecting each endpoint than to the shape of the dose-response curve.

The highest concentrations of herbicides measured in flowing surface waters are often only present for short periods of time. These herbicide pulses can reach concentrations that would affect aquatic plants if present over a long time. The aim of this study was to assess the effect of a 3-h herbicide pulse relative to the effects of long-term (4 and 7 days) exposure of six herbicides with different sites of action and different K(ow) on the growth of the floating macrophyte Lemna minor. The herbicides were the two photosynthetic inhibitors: diquat and terbuthylazine, the inhibitors of acetolactate syntase (ALS), imazamox and metsulfuron-methyl and the microtubule assembly inhibitors propyzamide and pendimethalin. The log K(ow) ranged from -4.6 to 5.2. For imazamox, metsulfuron-methyl, propyzamide and pendimethalin a 3-h pulse induced the effect on area-specific growth as did a 4-day exposure at an approximate 10-fold higher concentration. For diquat and terbuthylazine a concentration closer to a factor of 100 or more was needed for a 3-h pulse to induce an effect similar to that of a 4-day exposure. For diquat, the low pulse-effect was most likely due to a slow uptake of the hydrophilic ion (log K(ow) = -4.6), as no effect was observed on chlorophyll fluorescence within 8 h after exposure. The chlorophyll fluorescence parameters are expected to respond quickly to a PSI inhibitor as diquat. For terbuthylazine, fluorescence measurements showed an effect on photosynthesis within 1h of exposure, and reached a minimum after 3 h. Recovery was fast, and initial fluorescence was restored within 24 h. Hence, the small pulse effect on area-specific growth was due to rapid recovery of photosynthesis. In contrast to terbuthylazine, the stop in area-specific growth observed for the ALS-and microtubule assembly inhibitors, took up to 4 days to recover from. Such a long recovery time after a pulse of only 3 h indicate that at realistic pulse exposures of up to a day or two, pulse-effects will approach the effects obtained in long-term studies. When investigating the effects of pulse exposures on aquatic plants, we should therefore focus more on non-photosynthetic inhibitors, which might not appear in pulses in as large concentrations as the PSII inhibitors investigated up till now, but whose effect, even in a shorter pulse, can be more damaging.

The s-triazine herbicide terbutylazine, an inhibitor of photosystem II, is often found in surface waters in concentrations < 1 microg L(-1), but concentrations up to 13 microg L(-1) have been measured. To study the effect on the aquatic flora, we tested the sensitivity of 10 aquatic macrophyte species and a natural epiphyte community in a 2-week laboratory multispecies test at constant terbutylazine concentrations and two irradiance regimes. The data were described by a log-logistic concentration-response model and species sensitivity distributions (SSDs) were created from the EC50 and EC10 values. The 5% hazard concentration (HC5) of the EC10-based SSD for terbutylazine was 1 and 3 microg L(-1); hence the low chronic terbutylazine concentrations measured in the environment are not likely to affect the macrophyte community. To compare the species sensitivity between different groups of herbicides, SSDs were constructed from a published study on the sulfonylurea metsulfuron-methyl, an inhibitor of acetolactate synthase. There was no correlation between species-specific sensitivity to the two herbicides; hence, the combined exposure of different herbicides might affect the macrophyte community more broadly rather than seriously affecting a few susceptible species. Evaluating the standard procedure of leaving at least a factor of 100 between the EC50 of standard tests on Lemna sp. and the predicted environmental concentration seems to be protective for at least 95% of the macrophyte species for both terbutylazine and metsulfuron-methyl.

A suite of dose-response bioassays with white mustard (Sinapis alba L) and sugar beet (Beta vulgaris L) in the greenhouse and with three herbicides was used to analyse how the fluorescence induction curves (Kautsky curves) were affected by the herbicides. Bentazone, a photosystem II (PSII) inhibitor, completely blocked the normal fluorescence decay after the P-step. In contrast, fluorescence decay was still obvious for flurochloridone, a PDS inhibitor, and glyphosate, an EPSP inhibitor, which indicated that PSII inhibition was incomplete. From the numerous parameters that can be derived from OJIP-steps of the Kautsky curve the relative changes at the J-step [Fvj = (Fm - Fj)/Fm] was selected to be a common response parameter for the herbicides and yielded consistent dose-response relationships. Four hours after treatment, the response Fvj on the doses of bentazone and flurochloridone could be measured. For glyphosate, the changes of the Kautsky curve could similarly be detected 4 h after treatment in sugar beet, but only after 24 hs in S alba. The best prediction of biomass in relation to Fvj was found for bentazone. The experiments were conducted between May and August 2002 and showed that the ambient temperature and solar radiation in the greenhouse could affect dose-response relationships. If the Kautsky curve parameters should be used to predict the outcome of herbicide screening experiments in the greenhouse, where ambient radiation and temperature can only partly be controlled, it is imperative that the chosen fluorescence parameters can be used to predict accurately the resulting biomass used in classical bioassays.

An analytical method is described for the extraction of metsulfuron-methyl from soil at sub-parts per billion levels (LOQ = 0.2 microgram kg(-1)). The herbicide was quantitatively determined and identified by ESI LC/MS/MS. The method has been applied to a field dissipation study in which metsulfuron-methyl was applied to spring barley at three dosage rates: 4, 8, and 16 g of active ingredient ha(-)(1). The results of 2 years are presented. The dissipation rate of metsulfuron-methyl in topsoil was very rapid, with a calculated half-life of 6.5 days. Laboratory mineralization studies with native soils in contrast to autoclaved soils indicated that microbial degradation of (14)C-labeled metsulfuron-methyl and (14)C-labeled 2-amino-4-methoxy-6-methyl-1,3,5-triazine in soil microcosms is an important factor for the complete degradation of metsulfuron-methyl in the field. However, the mineralization rate of the sulfonamide was much higher.