Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis
Конференцијски прилог (Објављена верзија)
Метаподаци
Приказ свих података о документуАпстракт
Chlorpyrifos is one of organophosphorus (OPPs) insecticides, which are the most important and widely used classes of agricultural pesticides. Because of its intensive use of ecosystems are contaminated by chlorpyrifos and public concerns on safety have been increased.
The method has been developed for confirmation and quantitation of the chlorpyrifos in water samples reverse phase high performance liquid chromatography (HPLC) with photodiodes detection and chromatograms were extracted at 300 nm. This method was single-lab validate in order to demonstrate its performance for monitoring of the insecticide chlorpyrifos in water.
Method accuracy was quantified through measurement uncertainty estimate based on method validation data. Tap and groundwater samples were used to demonstrate linearity and accuracy. Linearity for chlorpyrifos was evaluated by calibration curves in the range of 0.01—10 pg/ml. The accuracy of the proposed method was evaluated as the mean recovery. The analytical m...ethod allowed us to quantify chlorpyrifos in tap water and groundwater in concentration level between 0.01-—10 pg/ml with recovery values between of 80.72-109.57 % for tap water and 89.99-97.45 % for groundwater and repeatability lower or equal than 0.6% for both the matrices. The experiments showed that there were no interference peaks from the water matrix (tap and ground) on the elution region of the chlorpyrifos. The RSD values were satisfactory being in the ranges of 0.283-1.237 % (for tap water) and 0.681-3.887 % (for groundwater). The variation of the retention time was less than 0.05 % during these experimental series. The combined relative uncertainty for water samples was 0.481 % (for tap water) and 0.654 % (for groundwater). The expanded uncertainty (Uc) was calculated as Uc= k*u,, where k is the coverage factor with level of confidence of approximately 95% considering a coverage factor of 2 (EURACHEMICITAC, 2000).
We proved that the method was specific for determination of chlorpyrifos in the relevant matrices. After validation and measurement uncertainty evaluation steps, results obtained showed that the method can be applied to efficiently for monitoring of chlorpyrifos in water samples.
Кључне речи:
insecticides / water / method validation / chlorpyrifos / organophosphorus pesticidesИзвор:
Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012, 2012, 73-73Издавач:
- Beograd : Društvo za zaštitu bilja Srbije
Финансирање / пројекти:
- Унапређење ремедијационих технологија и развој метода за процену ризика загађених локалитета (RS-MESTD-Integrated and Interdisciplinary Research (IIR or III)-43005)
- Стање, тенденције и могућности повећања плодности пољопривредног земљишта у Војводини (RS-MESTD-Technological Development (TD or TR)-31072)
Колекције
Институција/група
FiVeRTY - CONF AU - Lazić, S. AU - Grahovac, Nada AU - Šunjka, D. AU - Pucarevic, M. AU - Jakšić, Snežana AU - Popović, Vera PY - 2012 UR - http://fiver.ifvcns.rs/handle/123456789/3726 AB - Chlorpyrifos is one of organophosphorus (OPPs) insecticides, which are the most important and widely used classes of agricultural pesticides. Because of its intensive use of ecosystems are contaminated by chlorpyrifos and public concerns on safety have been increased. The method has been developed for confirmation and quantitation of the chlorpyrifos in water samples reverse phase high performance liquid chromatography (HPLC) with photodiodes detection and chromatograms were extracted at 300 nm. This method was single-lab validate in order to demonstrate its performance for monitoring of the insecticide chlorpyrifos in water. Method accuracy was quantified through measurement uncertainty estimate based on method validation data. Tap and groundwater samples were used to demonstrate linearity and accuracy. Linearity for chlorpyrifos was evaluated by calibration curves in the range of 0.01—10 pg/ml. The accuracy of the proposed method was evaluated as the mean recovery. The analytical method allowed us to quantify chlorpyrifos in tap water and groundwater in concentration level between 0.01-—10 pg/ml with recovery values between of 80.72-109.57 % for tap water and 89.99-97.45 % for groundwater and repeatability lower or equal than 0.6% for both the matrices. The experiments showed that there were no interference peaks from the water matrix (tap and ground) on the elution region of the chlorpyrifos. The RSD values were satisfactory being in the ranges of 0.283-1.237 % (for tap water) and 0.681-3.887 % (for groundwater). The variation of the retention time was less than 0.05 % during these experimental series. The combined relative uncertainty for water samples was 0.481 % (for tap water) and 0.654 % (for groundwater). The expanded uncertainty (Uc) was calculated as Uc= k*u,, where k is the coverage factor with level of confidence of approximately 95% considering a coverage factor of 2 (EURACHEMICITAC, 2000). We proved that the method was specific for determination of chlorpyrifos in the relevant matrices. After validation and measurement uncertainty evaluation steps, results obtained showed that the method can be applied to efficiently for monitoring of chlorpyrifos in water samples. PB - Beograd : Društvo za zaštitu bilja Srbije C3 - Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012 T1 - Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis EP - 73 SP - 73 UR - https://hdl.handle.net/21.15107/rcub_fiver_3726 ER -
@conference{ author = "Lazić, S. and Grahovac, Nada and Šunjka, D. and Pucarevic, M. and Jakšić, Snežana and Popović, Vera", year = "2012", abstract = "Chlorpyrifos is one of organophosphorus (OPPs) insecticides, which are the most important and widely used classes of agricultural pesticides. Because of its intensive use of ecosystems are contaminated by chlorpyrifos and public concerns on safety have been increased. The method has been developed for confirmation and quantitation of the chlorpyrifos in water samples reverse phase high performance liquid chromatography (HPLC) with photodiodes detection and chromatograms were extracted at 300 nm. This method was single-lab validate in order to demonstrate its performance for monitoring of the insecticide chlorpyrifos in water. Method accuracy was quantified through measurement uncertainty estimate based on method validation data. Tap and groundwater samples were used to demonstrate linearity and accuracy. Linearity for chlorpyrifos was evaluated by calibration curves in the range of 0.01—10 pg/ml. The accuracy of the proposed method was evaluated as the mean recovery. The analytical method allowed us to quantify chlorpyrifos in tap water and groundwater in concentration level between 0.01-—10 pg/ml with recovery values between of 80.72-109.57 % for tap water and 89.99-97.45 % for groundwater and repeatability lower or equal than 0.6% for both the matrices. The experiments showed that there were no interference peaks from the water matrix (tap and ground) on the elution region of the chlorpyrifos. The RSD values were satisfactory being in the ranges of 0.283-1.237 % (for tap water) and 0.681-3.887 % (for groundwater). The variation of the retention time was less than 0.05 % during these experimental series. The combined relative uncertainty for water samples was 0.481 % (for tap water) and 0.654 % (for groundwater). The expanded uncertainty (Uc) was calculated as Uc= k*u,, where k is the coverage factor with level of confidence of approximately 95% considering a coverage factor of 2 (EURACHEMICITAC, 2000). We proved that the method was specific for determination of chlorpyrifos in the relevant matrices. After validation and measurement uncertainty evaluation steps, results obtained showed that the method can be applied to efficiently for monitoring of chlorpyrifos in water samples.", publisher = "Beograd : Društvo za zaštitu bilja Srbije", journal = "Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012", title = "Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis", pages = "73-73", url = "https://hdl.handle.net/21.15107/rcub_fiver_3726" }
Lazić, S., Grahovac, N., Šunjka, D., Pucarevic, M., Jakšić, S.,& Popović, V.. (2012). Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis. in Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012 Beograd : Društvo za zaštitu bilja Srbije., 73-73. https://hdl.handle.net/21.15107/rcub_fiver_3726
Lazić S, Grahovac N, Šunjka D, Pucarevic M, Jakšić S, Popović V. Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis. in Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012. 2012;:73-73. https://hdl.handle.net/21.15107/rcub_fiver_3726 .
Lazić, S., Grahovac, Nada, Šunjka, D., Pucarevic, M., Jakšić, Snežana, Popović, Vera, "Method validation and uncertainty evaluation of the insecticide chlorpyrifos in water samples by using HPLC analysis" in Annual MGPR Meeting 2012 and International Conference on Food and Health Safety: Moving Towards a Sustainable Agriculture, Belgrade, 11 October 2012 (2012):73-73, https://hdl.handle.net/21.15107/rcub_fiver_3726 .