Method development for monitoring pesticides in environmental waters: liquid-solid extraction followed by liquid chromatography

Corcia, Antonio Di; Marchetti, M. C.

doi:10.1021/es00025a004

Cited by 180 publications

(69 citation statements)

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“…Solid-phase extraction (SPE) was developed to overcome these problems and has been successfully used for the analysis of organic micro-pollutants in water [16][17][18][19][20][21]. The technique is based on the principle of gassolid adsorption for sampling and liquid -solid chromatography for extraction.…”

Section: T} Dedicated To Michele DI Pasquale (Deceased)mentioning

confidence: 99%

Fast determination of VOCs in workplace air by solid-phase extraction and gas chromatography-mass spectrometry

1998

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Section: T} Dedicated To Michele DI Pasquale (Deceased)mentioning

confidence: 99%

Fast determination of VOCs in workplace air by solid-phase extraction and gas chromatography-mass spectrometry

1998

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“…In reversedphase chromatography, it is well known that hydrophobic compounds are well retained by these sorbents in water as mobile phase and that their sep a ration re q u i res a mobile phase containing an organic solvent whereas polar analytes are difficult to be retained and separated with an aqueous mobile phase. The limitation of using n-a l kyl silicas will therefore occur for the more polar pesticides and degradation products [1,2,[7][8][9][10][11]. For very apolar analytes, one has just to take care of avoiding losses by adsorption on flasks and connection tubes which can be solved by the addition of some organic solvent before the percolation of samples through the extraction device [12,13].…”

Section: N-alkyl Silicasmentioning

confidence: 99%

“…Their higher efficiency over C 18 silica for trapping polar pesticides have been extensively shown by the group of Di Corcia et al [1,[25][26][27][28]. GCB are not enough pressure resistant to be used in LC so that no data indicating the LC behaviour of solutes are available.…”

Section: Carbonaceous Sorbentsmentioning

confidence: 99%

“…Liquid chromatography have been shown to be suitable for mu l t i residue sep a ration of many compounds over a wide ra n ge of polarity without prev i o u s derivatization. Examples can be found in the literature, the most impressive one being the multiresidue separation of 72 pesticides in one run published by Di Corcia and Marchetti some time ago [1]. However, despite the advances in separation and quantifi c ation tech n i q u e s , no sample can be directly analyzed and a multiresidue extraction is a compulsory step in the analytical procedure.…”

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Multiresidue solid-phase extraction for trace-analysis of pesticides and their metabolites in environmental water

Pichon¹

1998

Analusis

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Recent research on the fate and transformation of pesticides in the environment has pointed out the need for including more and more polar analytes in multiresidue analysis. Liquid chromatography have been shown to be suitable for mu l t i residue sep a ration of many compounds over a wide ra n ge of polarity without prev i o u s derivatization. Examples can be found in the literature, the most impressive one being the multiresidue separation of 72 pesticides in one run published by Di Corcia and Marchetti some time ago [1]. However, despite the advances in separation and quantifi c ation tech n i q u e s , no sample can be directly analyzed and a multiresidue extraction is a compulsory step in the analytical procedure.In recent years, enrichment of trace compounds on suitable sorbents has been shown to be an interesting alternative to LLE, and has now become a reliable and useful tool for sample handling. In addition, many modern pesticides and identified degra d ation products are fa i rly soluble in water and are therefore less amenable to solvent extraction. Automation and new trends in SPEThe solid-phase extraction (SPE) area has been very active these past years, certainly due to the now well-recognized trends for using solvent-free methods in environmental analytical laboratories and for its suitability to automation [2]. The four individual steps of a typical SPE sequence-i) conditioning of the sorbent, ii) application of the sample, iii) rinsing and cleaning of the sample, and iv) desorption and recovery of the analytes to be separated-can be performed sequentially for up to 24 cartridges at the same time using extraction units working under positive or negative pressure. The whole sequence can also be easily automated with devices now available by several companies using any comm e rcial cart ri d ges or ex t raction disks. Examples are the ASPEC from Gilson, Microlab from Hamilton, AutoTrace and RapidTrace from Zymark. Possibility exists for some of these devices for automatic injection of an aliquot of the final extract into the chromatographic system. The complete automation also exists which couples SPE with direct online LC analysis (ASPEC XL from Gilson, Prospekt from Spark Holland, OSP-2 from Merck). These last two apparatus improved productivity since the next sample is automatically prepared while the previous sample is being analyzed. Th e re fo re, method development can easily be automat e d with various degrees of automation.Off-line SPE materials are mainly disposable cartridges and disk membranes. Besides automation, two other main SPE characteristics have been commercially developed. The first one tends to increase the sample thoughput and the second one to broaden the polarity range of analytes to extract. R e s t ricted fl ow rates and cl ogging are often observe d when handling water containing suspended solids such as surface water. Various approaches have been developed to solve this problem. One consists in depth filters which can be placed above the cartridge or membrane extracti...

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“…Several techniques for multiresidue pesticide analysis in natural waters have been applied to environmental samples in recent years, including solid phase extraction (SPE)-GC-MS [3,4], SPE-HPLC [5,6] or LC-MS [7][8][9][10].…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of base/neutral and acid herbicides in natural water at the part per trillion level

et al. 1998

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A new method for the simultaneous identification and quantification of base/neutral and acidic pesticides at a low nanogram per liter concentration level in natural waters is presented. The method includes enrichment of the compounds by solid phase extraction on graphitized carbon black, followed by sequential elution of the base/neutral and acidic pesticides. Identification and quantification of the compounds is performed with HPLC-ESI-MS. This procedure involves passing 1 L of ground water and 2 L of drinking water samples through a 0.5 g graphitized carbon black (GCB) extraction cartridge. A conventional 4.6-mm-i.d. reversed phase LC C-18 operating with a 1 mt min-l flow of the mobile phase was used to chromatograph the analytes. A flow of 100 mu L min(-1) of the column effluent was diverted to the ESI source. The ESI source was operated in positive ion mode for base/neutral pesticides and in negative-ion mode for acid pesticides. For the analyte considered, the response of the mass detector was linearly related to the amount of the analytes injected between 5 and 250 ng. In all cases, recoveries of the analytes were better than 90%. The limit of detection (signal-to-noise ratio = 3) of the method for the pesticides considered in drinking water samples was estimated to be about 3-10 ng L-1

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Method development for monitoring pesticides in environmental waters: liquid-solid extraction followed by liquid chromatography

Cited by 180 publications

References 11 publications

Fast determination of VOCs in workplace air by solid-phase extraction and gas chromatography-mass spectrometry

Fast determination of VOCs in workplace air by solid-phase extraction and gas chromatography-mass spectrometry

Multiresidue solid-phase extraction for trace-analysis of pesticides and their metabolites in environmental water

Simultaneous determination of base/neutral and acid herbicides in natural water at the part per trillion level

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