Salting-Out Assisted Liquid-Liquid Extraction Combined with HPLC for Quantitative Extraction of Trace Multiclass Pesticide Residues from Environmental Waters

In this study, salting-out assisted liquid-liquid extraction combined with high performance liquid chromatography diode array detector (SALLE-HPLC-DAD) method was developed and validated for simultaneous analysis of carbaryl, atrazine, propazine, chlorothalonil, dimethametryn and terbutryn in environmental water samples. Parameters affecting the extraction efficiency such as type and volume of extraction solvent, sample volume, salt type and amount, centrifugation speed and time, and sample pH were optimized. Under the optimum extraction conditions the method was linear over the range of 10 - 100 μg/L (carbaryl), 8 - 100 μg/L (atarzine), 7 - 100 μg/L (propazine) and 9 - 100 μg/L (chlorothalonil, terbutryn and dimethametryn) with correlation coefficients (R2) between 0.99 and 0.999. Limits of detection and quantification ranged from 2.0 to 2.8 μg/L and 6.7 to 9.5 μg/L, respectively. The extraction recoveries obtained for ground, lake and river waters were in a range of 75.5% to 106.6%, with the intra-day and inter-day relative standard deviation lower than 3.4% for all the target analytes. All of the target analytes were not detected in these samples. Therefore, the proposed SALLE-HPLC-DAD method is simple, rapid, cheap and environmentally friendly for the determination of the aforementioned herbicides, insecticide and fungicide residues in environmental water samples.

[1]  A. Fernandez-Gutiérrez,et al.  Multiresidue analysis of phenylurea herbicides in environmental waters by capillary electrophoresis using electrochemical detection , 2005, Analytical and bioanalytical chemistry.

[2]  P. Sandra,et al.  Dual-phase twisters: a new approach to headspace sorptive extraction and stir bar sorptive extraction. , 2005, Journal of chromatography. A.

[3]  M. Biziuk,et al.  Determination of organophosphorus and organonitrogen pesticides in water samples , 2010 .

[4]  Carolina Quesada-Molina,et al.  Trace determination of sulfonylurea herbicides in water and grape samples by capillary zone electrophoresis using large volume sample stacking , 2010, Analytical and bioanalytical chemistry.

[5]  N. Retta,et al.  Ion-pair assisted liquid–liquid extraction for selective separation and analysis of multiclass pesticide residues in environmental waters , 2014 .

[6]  Shibin Hu,et al.  Salting-out assisted liquid-liquid extraction coupled to dispersive liquid-liquid microextraction for the determination of chlorophenols in wine by high-performance liquid chromatography. , 2014, Journal of separation science.

[7]  M. Jiang,et al.  Miniaturized salting-out liquid-liquid extraction of sulfonamides from different matrices. , 2010, Analytica chimica acta.

[8]  Negussie Megersa.  Hollow fiber-liquid phase microextraction for trace enrichment of the residues of atrazine and its major degradation products from environmental water and human urine samples , 2015 .

[9]  Negussie Megersa,et al.  Low density solvent based dispersive liquid-liquid microextraction and preconcentration of multiresidue pesticides in environmental waters for liquid chromatographic analysis , 2015, Journal of Analytical Chemistry.

[10]  D. Djozan,et al.  Development of a new dispersive liquid-liquid microextraction method in a narrow-bore tube for preconcentration of triazole pesticides from aqueous samples. , 2012, Analytica chimica acta.

[11]  Francisco J. Lara,et al.  Hollow-fiber liquid-phase microextraction combined with capillary HPLC for the selective determination of six sulfonylurea herbicides in environmental waters. , 2013, Journal of separation science.

[12]  P. C. Kearney,et al.  Herbicides: Chemistry, Degradation, and Mode of Action , 1976 .

[13]  Á. Ríos,et al.  Ionic liquids supported on magnetic nanoparticles as a sorbent preconcentration material for sulfonylurea herbicides prior to their determination by capillary liquid chromatography , 2012, Analytical and Bioanalytical Chemistry.

[14]  R. Plantier-Royon,et al.  Removal of pesticides from wastewater by ion pair Centrifugal Partition Extraction using betaine-derived ionic liquids as extractants , 2016 .

[15]  Chun Wang,et al.  Dispersive Solid-Phase Extraction Clean-up Combined with Dispersive Liquid–Liquid Microextraction for the Determination of Neonicotinoid Insecticides in Vegetable Samples by High-Performance Liquid Chromatography , 2011 .

[16]  J. P. Pavón,et al.  In situ aqueous derivatization and determination of non-steroidal anti-inflammatory drugs by salting-out-assisted liquid-liquid extraction and gas chromatography-mass spectrometry. , 2011, Journal of chromatography. A.

[17]  Lingxin Chen,et al.  Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography. , 2013, Talanta.

[18]  R. Zhao,et al.  Sensitive determination of amide herbicides in environmental water samples by a combination of solid-phase extraction and dispersive liquid-liquid microextraction prior to GC-MS. , 2009, Journal of separation science.

[19]  J. Namieśnik,et al.  Advances in passive sampling in environmental studies. , 2007, Analytica chimica acta.

[20]  Mohammad Rezaee,et al.  Evolution of dispersive liquid-liquid microextraction method. , 2010, Journal of chromatography. A.

[21]  B. Hauser,et al.  Membrane-assisted solvent extraction of triazines, organochlorine, and organophosphorus compounds in complex samples combined with large-volume injection-gas chromatography/mass spectrometric detection. , 2004, Analytical chemistry.

[22]  Negussie Megersa,et al.  Salting-out-assisted liquid–liquid extraction for the preconcentration and quantitative determination of eight herbicide residues simultaneously in different water samples with high-performance liquid chromatography , 2017 .

[23]  Ann B. Strong,et al.  Comparison of solid phase extraction with salting-out solvent extraction for preconcentration of nitroaromatic and nitramine explosives from water , 1994 .

[24]  O. Thomas,et al.  Effect of Endocrine Disruptor Pesticides: A Review , 2011, International journal of environmental research and public health.

[25]  N. Regassa,et al.  Impacts of improved seeds and agrochemicals on food security and environment in the Rift Valley of Ethiopia: implications for the application of an African green revolution , 2010 .

[26]  Sergio C. Nanita,et al.  Ammonium chloride salting out extraction/cleanup for trace-level quantitative analysis in food and biological matrices by flow injection tandem mass spectrometry. , 2013, Analytica chimica acta.

[27]  A. Daneshfar,et al.  Determination of methylene blue and sunset yellow in wastewater and food samples using salting-out assisted liquid-liquid extraction , 2011 .

[28]  C. Kerr,et al.  Simultaneous extraction and determination of various pesticides in environmental waters. , 2014, Journal of separation science.

[29]  Huaiqin Wu,et al.  Salting-out assisted liquid/liquid extraction with acetonitrile: a new high throughput sample preparation technique for good laboratory practice bioanalysis using liquid chromatography-mass spectrometry. , 2009, Biomedical chromatography : BMC.

[30]  Á. Ríos,et al.  Use of gold nanoparticle-coated sorbent materials for the selective preconcentration of sulfonylurea herbicides in water samples and determination by capillary liquid chromatography. , 2013, Talanta.

[31]  Yaqi Cai,et al.  A liquid–liquid extraction technique for phthalate esters with water-soluble organic solvents by adding inorganic salts , 2007 .

[32]  J. Jönsson,et al.  Trace enrichment and sample preparation of alkylthio-s-triazine herbicides in environmental waters using a supported liquid membrane technique in combination with high-performance liquid chromatography , 1998 .

[33]  M. Saraji,et al.  Application of dispersive liquid-liquid microextraction for the determination of phenylurea herbicides in water samples by HPLC-diode array detection. , 2009, Journal of separation science.

[34]  D. Karpouzas,et al.  Development and validation of an HPLC-DAD method for the simultaneous determination of most common rice pesticides in paddy water systems , 2012 .

[35]  L. Mathiasson,et al.  Assessment of organochlorine pesticide pollution in Upper Awash Ethiopian state farm soils using selective pressurised liquid extraction. , 2008, Chemosphere.

[36]  Negussie Megersa,et al.  Salting-out assisted liquid-liquid extraction combined with capillary HPLC for the determination of sulfonylurea herbicides in environmental water and banana juice samples. , 2014, Talanta.

[37]  M. Biziuk,et al.  Solventless and solvent-minimized sample preparation techniques for determining currently used pesticides in water samples: a review. , 2011, Talanta.

[38]  T. Albanis,et al.  Liquid-phase micro-extraction techniques in pesticide residue analysis. , 2007, Journal of biochemical and biophysical methods.

[39]  R. Jeannot,et al.  Multiresidue methods using solid-phase extraction techniques for monitoring priority pesticides, including triazines and degradation products, in ground and surface waters. , 2000, Journal of chromatography. A.

[40]  Jing-fu Liu,et al.  Development of a one-step microwave-assisted extraction method for simultaneous determination of organophosphorus pesticides and fungicides in soils by gas chromatography-mass spectrometry. , 2013, Talanta.

[41]  F. Gosetti,et al.  HPLC-UV and HPLC-MSn multiresidue determination of amidosulfuron, azimsulfuron, nicosulfuron, rimsulfuron, thifensulfuron methyl, tribenuron methyl and azoxystrobin in surface waters. , 2006, Analytica chimica acta.