Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection.
Аутори
Grahovac, NadaSuturović, Z.
Kondić-Špika, Ankica
Sekulić, Petar
Lazić, Sanja
Šunjka, Dragana
Jakšić, Snežana
Конференцијски прилог (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
Pesticides having different structures and biological activities are widely used for
agricultural and non-agricultural purposes. Due to their widespread use, pesticides neeq
to be determined in various environmental matrices, A wide range of analytical
techniques have been developed in order to identify the organic contaminants often
present at trace levels in environmental samples. The aim of this work was to develop a
reliable, rapid, robust and cost-effective method for the determination of five sulfonylurea
herbicides (nicosulfuron, oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) +
spiked river water samples. The samples were diluted with 0 5% acetic acid (1:1) an
purified by solid-phase extraction (SPE) on Oasis MAX cartridges. After the cartridges
were sequentially washed with water, methanol, ethyl acetate, and acetonitrile, they were
eluted with 0.1% formic acid in acetonitrile. Elutes were evaporated to dryness and
reconstituted in acetonitrile. The ...purified extracts were analyzed by reversed-phase highperformance liquid chromatography with diode-array detection (HPLC-DAD) system. The
best separation was achieved on a Zorbax Eclipse XDB-Cis (50mm x 4.6mm x 1.8m)
analytical column with gradient elution at a flow rate of 1 mL/min. The analyte was
monitored at 230 nm. The linearity of calibration curve within the tested concentration
range exhibited correlation coefficients (r) higher than 0.998. The accuracy of the
method was acceptable since the average recoveries measured at two fortification levels
were in the range of 92.5-97.5% (n=3). The precision of the developed procedure
expressed as the relative standard deviations (RSDs) were lower than 4.76% in all cases
The repeatability of the retention time and peak area was checked by injecting standard
solution ten times. The relative standard deviation of the retention time and the peak area
was found to be less than 0.2% and 0 6%, respectively. The method was also validated
by analyzing freshly spiked river water samples The proposed analytical method might
be successfully applied in monitoring of sulfonylurea herbicides (nicosulfuron,
oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) in surface water and
groundwater samples
Кључне речи:
sulfonylurea herbicides / determination / surface water / HPLC-DADИзвор:
Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens, 2013, 1-8Издавач:
- Athens : University of the Aegean
Финансирање / пројекти:
- Стање, тенденције и могућности повећања плодности пољопривредног земљишта у Војводини (RS-MESTD-Technological Development (TD or TR)-31072)
Колекције
Институција/група
FiVeRTY - CONF AU - Grahovac, Nada AU - Suturović, Z. AU - Kondić-Špika, Ankica AU - Sekulić, Petar AU - Lazić, Sanja AU - Šunjka, Dragana AU - Jakšić, Snežana PY - 2013 UR - http://fiver.ifvcns.rs/handle/123456789/3305 AB - Pesticides having different structures and biological activities are widely used for agricultural and non-agricultural purposes. Due to their widespread use, pesticides neeq to be determined in various environmental matrices, A wide range of analytical techniques have been developed in order to identify the organic contaminants often present at trace levels in environmental samples. The aim of this work was to develop a reliable, rapid, robust and cost-effective method for the determination of five sulfonylurea herbicides (nicosulfuron, oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) + spiked river water samples. The samples were diluted with 0 5% acetic acid (1:1) an purified by solid-phase extraction (SPE) on Oasis MAX cartridges. After the cartridges were sequentially washed with water, methanol, ethyl acetate, and acetonitrile, they were eluted with 0.1% formic acid in acetonitrile. Elutes were evaporated to dryness and reconstituted in acetonitrile. The purified extracts were analyzed by reversed-phase highperformance liquid chromatography with diode-array detection (HPLC-DAD) system. The best separation was achieved on a Zorbax Eclipse XDB-Cis (50mm x 4.6mm x 1.8m) analytical column with gradient elution at a flow rate of 1 mL/min. The analyte was monitored at 230 nm. The linearity of calibration curve within the tested concentration range exhibited correlation coefficients (r) higher than 0.998. The accuracy of the method was acceptable since the average recoveries measured at two fortification levels were in the range of 92.5-97.5% (n=3). The precision of the developed procedure expressed as the relative standard deviations (RSDs) were lower than 4.76% in all cases The repeatability of the retention time and peak area was checked by injecting standard solution ten times. The relative standard deviation of the retention time and the peak area was found to be less than 0.2% and 0 6%, respectively. The method was also validated by analyzing freshly spiked river water samples The proposed analytical method might be successfully applied in monitoring of sulfonylurea herbicides (nicosulfuron, oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) in surface water and groundwater samples PB - Athens : University of the Aegean C3 - Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens T1 - Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection. EP - 8 SP - 1 UR - https://hdl.handle.net/21.15107/rcub_fiver_3305 ER -
@conference{ author = "Grahovac, Nada and Suturović, Z. and Kondić-Špika, Ankica and Sekulić, Petar and Lazić, Sanja and Šunjka, Dragana and Jakšić, Snežana", year = "2013", abstract = "Pesticides having different structures and biological activities are widely used for agricultural and non-agricultural purposes. Due to their widespread use, pesticides neeq to be determined in various environmental matrices, A wide range of analytical techniques have been developed in order to identify the organic contaminants often present at trace levels in environmental samples. The aim of this work was to develop a reliable, rapid, robust and cost-effective method for the determination of five sulfonylurea herbicides (nicosulfuron, oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) + spiked river water samples. The samples were diluted with 0 5% acetic acid (1:1) an purified by solid-phase extraction (SPE) on Oasis MAX cartridges. After the cartridges were sequentially washed with water, methanol, ethyl acetate, and acetonitrile, they were eluted with 0.1% formic acid in acetonitrile. Elutes were evaporated to dryness and reconstituted in acetonitrile. The purified extracts were analyzed by reversed-phase highperformance liquid chromatography with diode-array detection (HPLC-DAD) system. The best separation was achieved on a Zorbax Eclipse XDB-Cis (50mm x 4.6mm x 1.8m) analytical column with gradient elution at a flow rate of 1 mL/min. The analyte was monitored at 230 nm. The linearity of calibration curve within the tested concentration range exhibited correlation coefficients (r) higher than 0.998. The accuracy of the method was acceptable since the average recoveries measured at two fortification levels were in the range of 92.5-97.5% (n=3). The precision of the developed procedure expressed as the relative standard deviations (RSDs) were lower than 4.76% in all cases The repeatability of the retention time and peak area was checked by injecting standard solution ten times. The relative standard deviation of the retention time and the peak area was found to be less than 0.2% and 0 6%, respectively. The method was also validated by analyzing freshly spiked river water samples The proposed analytical method might be successfully applied in monitoring of sulfonylurea herbicides (nicosulfuron, oxasulfuron, tribenuron methyl, triasulfuron and tritosulfuron) in surface water and groundwater samples", publisher = "Athens : University of the Aegean", journal = "Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens", title = "Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection.", pages = "8-1", url = "https://hdl.handle.net/21.15107/rcub_fiver_3305" }
Grahovac, N., Suturović, Z., Kondić-Špika, A., Sekulić, P., Lazić, S., Šunjka, D.,& Jakšić, S.. (2013). Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection.. in Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens Athens : University of the Aegean., 1-8. https://hdl.handle.net/21.15107/rcub_fiver_3305
Grahovac N, Suturović Z, Kondić-Špika A, Sekulić P, Lazić S, Šunjka D, Jakšić S. Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection.. in Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens. 2013;:1-8. https://hdl.handle.net/21.15107/rcub_fiver_3305 .
Grahovac, Nada, Suturović, Z., Kondić-Špika, Ankica, Sekulić, Petar, Lazić, Sanja, Šunjka, Dragana, Jakšić, Snežana, "Analytical method validation for the determination of sulfonylurea herbicides in water samples by solid-phase extraction and HPLC with diode-array detection." in Proceedings, 13th International Conference on Environmental Science and Technology (CEST2013), 5-7 September 2013, Athens (2013):1-8, https://hdl.handle.net/21.15107/rcub_fiver_3305 .