scholarly journals Comparison of Capillary Electrophoresis and Liquid Chromatography for Determination of Sulfonylurea Herbicides in Soil

1999 ◽  
Vol 82 (6) ◽  
pp. 1534-1541 ◽  
Author(s):  
Hubert J Menne ◽  
Karin Janowitz ◽  
Bernhard M Berger

Abstract Two analytical methods developed for degradation studies in soil were compared for the simultaneous determination of sulfonylurea herbicides. The compounds were extracted with phosphate buffer from soil samples after purification and enrichment steps by solid-phase extraction. Samples were analyzed by liquid chromatography (LC) or capillary electrophoresis (CE) with UV detection. Amidosulfuron, bensulfuron-methyl, chlorimuron-ethyl, chlorsulfuron, ethametsulfuron-methyl, metsulfuron-methyl, nicosulfuron, primisulfuron-methyl, sulfometuron-methyl, thifensulfuron-methyl, triasulfuron, and tribenuron-methyl were separated within 90 and 35 min by LC and CE, respectively. Average recoveries, determined with LC for 5 sulfonylureas in 1–100 μg/kg soil ranged from 74 to 103%, and those determined with CE for 10 sulfonylureas in 2-20 μg/kg soil ranged from 87 to 105%. Bensulfuron-methyl was recovered at lower levels of 52%. The limits of quantitation were 1.0 and 2.0 μg/kg soil for LC and CE, respectively. Coefficients of variation were higher for CE than for LC. Although both methods are suitable, the LC method, which is more sensitive and accurate than the CE method, is preferred for field studies. However, CE, which was shown to be faster with lower operating costs and unlimited repeatability of the analysis due to little injection volumes, is preferred for laboratory studies.

2008 ◽  
Vol 1 (2) ◽  
pp. 161-166 ◽  
Author(s):  
A. Veršilovskis ◽  
S. De Saeger ◽  
V. Mikelsone

A new method for the determination of sterigmatocystin in beer was developed. This method consists of a solid phase extraction procedure of light and dark beer and reversed phase high performance liquid chromatography with ultraviolet detection. Recoveries of sterigmatocystin from beer samples spiked at levels from 0.5 to 100 µg/l ranged from 81 to 126% for light beer and from 88 to 126% for dark beer with coefficients of variation between 2.2 and 14%. From the total of 26 analysed Latvian beer samples only two (7.7%) were contaminated with sterigmatocystin.


1999 ◽  
Vol 82 (6) ◽  
pp. 1474-1478 ◽  
Author(s):  
Yoshie Yamazaki ◽  
Takahiro Ninomiya

Abstract A simple and rapid method was developed for determination of benomyl, diphenyl (DP), o-phenylphenol (OPP), thiabendazole (TBZ), chlorpyrifos, methidathion, and methyl parathion in whole oranges. These compounds were extracted from a mixture of samples and anhydrous sodium acetate with ethyl acetate. The ethyl acetate extract was concentrated and cleaned up by passing through tandem solid-phase extraction columns consisting of anion-exchange and primary/secondary amine bonded silica. The eluate was concentrated and volume was adjusted with methanol for subsequent liquid chromatography (LC) and gas chromatography (GC). Benomyl (as methyl-2-benzimidazole carbamate, MBC), DP, OPP, and TBZ residues were determined by LC with fluorescence detection. Recoveries at 3 fortified levels (0.1,1, and 10 μg/g) ranged from 63.9 to 97.4 %, with coefficients of variation (CVs) of 1.6 to 15.5 %. Limits of detection (LODs) were 0.01 μg/g for DP, OPP, TBZ and 0.05 μg/g for benomyl. Chlorpyrifos, methidathion, and methyl parathion residues were determined by GC with flame photometric detection. Recoveries ranged from 90.4 to 97.0 %, with CVs of 2.1 to 5.9 %. LODs were 0.005 μg/g for chlorpyrifos and methyl parathion, and 0.01 μg/g for methidathion.


1996 ◽  
Vol 79 (5) ◽  
pp. 1062-1068 ◽  
Author(s):  
Junsuo Li ◽  
Chuanfan Qian

Abstract A simple and specific procedure for determination of avermectin B1 in biological samples is described. A specific anti-avermectin B1 immunosorbent was developed. Avermectin B1 was extracted from cattle plasma, cattle meat, and pear samples. The extracts were cleaned up on a solid-phase extraction column (C18) and an immunoaffinity column. Avermectin B1 was determined by reversedphase liquid chromatography with UV detection at 245 nm. Recoveries of avermectin Bi from samples spiked at levels of 6 and 60 parts per billion (ppb) ranged from 80 to 86%, with coefficients of variation of 5-14%. The limit of detection was 2 ppb. The procedure provides a simple and sensitive method for monitoring avermectin B1 residues in biological matrixes.


1997 ◽  
Vol 80 (2) ◽  
pp. 392-400 ◽  
Author(s):  
Alexander J Krymtsky

Abstract A capillary electrophoresis (CE) method and an electrospray ionization (ESI) liquid chromatography/mass spectrometry (LC/MS) confirmatory method were developed to analyze 12 sulfonylurea herbicides and one sulfonamide (Flumetsulam) in runoff water. The water used for fortification was collected from a local marsh that contained high levels of potentially interfering compounds. Good recoveries and adequate sensitivity at the 0.2 ppb level (limit of quantitation) were obtained. A portion of the water was acidified and extracted with reversed- phase solid-phase extraction (SPE). Extracts were cleaned up with a tandem system consisting of a strong-anion exchange SPE cartridge stacked on an alumina SPE cartridge. CE/ultraviolet quantitation was achieved by capillary zone electrophoresis at pH 4.75 with 50 mM ammonium acetate buffer and an acetonitrile modifier. ESI LC/MS quantitation was achieved by using a time-scheduled selective-ion monitoring (positive mode) of the M+H ions for each compound. The extraction/cleanup procedure provided extracts such that in-source collision-induced dissociation gave product ions for confirmation at the 0.2 ppb fortification level.


2006 ◽  
Vol 89 (6) ◽  
pp. 1635-1640 ◽  
Author(s):  
Ji-Ye Hu ◽  
Jian-Zhong Li

Abstract A method using solid-phase extraction for cleanup, followed by high-performance liquid chromatography with ultraviolet detection (HPLC/UV), was developed for the determination of forchlorfenuron residues in watermelon. The pesticide is extracted from the sample with acidic acetonitrile, and the extract is loaded onto a primary-secondary amine (PSA) column. The pesticide is eluted with acetone and determined by HPLC/UV. The PSA column was found to provide effective cleanup, removing the greatest number of sample matrix interferences. The acetonitrile extraction followed by the PSA cleanup provided recoveries of >95%, coefficients of variation (precision) of <10%, and sensitivity of 0.005 mg/kg, in agreement with the directives for method validation in residue analysis. The proposed method was successfully used to determine forchlorfenuron residue levels and dissipation rates in watermelon grown in an experimental greenhouse in Beijing, People's Republic of China.


1999 ◽  
Vol 82 (6) ◽  
pp. 1523-1533 ◽  
Author(s):  
Heidi Hickes ◽  
Matthew Watrous

Abstract A liquid chromatographic method with comfirmation by capillary electrophoresis was used to determine 12 sulfonylurea herbicides in agricultural water. Analysis of 3 different water matrixes fortified at 2 levels gave good recoveries with adequate sensitivity at the 0.1 ppb level. A portion of the water was acidified with acetic acid and loaded onto an RP-102 solid-phase extraction (SPE) cartridge, and the extract was cleaned up on an alumina SPE cartridge. Extracts were desalted with an RP-102 SPE cartridge before instrumentation. Samples needing chemical filtration, such as pond water, required additional cleanup with a SAX SPE cartridge before the alumina cleanup step. Data were compiled for both determinative techniques and evaluated.


Sign in / Sign up

Export Citation Format

Share Document