Screening of Organochlorine Pesticide and Polychlorinated Biphenyl Residues in Nonfatty Seafood Products by Tandem Solid-Phase Extraction Cleanup

1994 ◽  
Vol 77 (1) ◽  
pp. 102-106 ◽  
Author(s):  
Frank J Schenck ◽  
Roberta Wagner ◽  
Michael K Hennessy ◽  
Joseph L Okrasinski
Keyword(s):  
Solid Phase Extraction ◽  
Organochlorine Pesticide ◽  
Polychlorinated Biphenyl ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Phase Extraction ◽  
Matrix Interferences ◽  
Seafood Products ◽  
Aoac Method ◽  
Spe Method

Abstract A rapid multiresidue solid-phase extraction (SPE) technique for the isolation and subsequent gas chromatographic (GC) determination of organo-chlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish, crabmeat, shrimp, and scallops is described. Samples are extracted with acetonitrile, and the extract is subjected to a cleanup using both C18 and Florisil SPE columns. The residues are determined by GC with electron capture detection. Because the injected extracts are free from matrix interferences, the amount of residue present is easily calculated. The average recoveries of 9 spiked (0.01–0.40 ppm) organo-chlorine pesticide residues from 6 different seafood products ranged from 93.8 to 98.4%. The average recoveries of spiked (0.50 ppm) PCB mixtures from 4 different seafood products ranged from 88.5 to 107.2%. This SPE method and the AOAC multiresidue method for organochlorine residues in fish produced comparable results for nonfatty seafood samples containing incurred organochlorine pesticide and PCB residues. The SPE method reduces organic solvent consumption by 95% and hazardous waste by 85% compared with the AOAC method. We were able to carry 10 seafood samples through the extraction and cleanup in less than 2 h by using the SPE method.

scholarly journals Determination of Organochlorine Pesticide and Polychlorinated Biphenyl Residues in Fatty Fish by Tandem Solid-Phase Extraction Cleanup

1996 ◽  
Vol 79 (5) ◽  
pp. 1209-1214 ◽  
Author(s):  
Frank J Schenck ◽  
Lori Calderon ◽  
Lynda V Podhorniak
Keyword(s):  
Solid Phase Extraction ◽  
Organochlorine Pesticide ◽  
Pesticide Residues ◽  
Polychlorinated Biphenyl ◽  
Solid Phase ◽  
Electron Capture Detection ◽  
Phase Extraction ◽  
Fatty Fish ◽  
Organochlorine Pesticide Residues

Abstract A rapid, multiresidue solid-phase extraction (SPE) technique for determination of organochlorine pesticide and polychlorinated biphenyl (PCB) residues in nonfatty fish was modified for use with fatty fish. In the modified procedures, samples are extracted with acetonitrile, and the extract is cleaned up with both C18 and Florisil SPE columns. Residues are determined by gas chromatography with electron capture detection. The original method was modified for use with fatty fish by reducing the amount of tissue extracted and by using an improved Florisil SPE cleanup. Recovery data are presented for 24 fortified organochlorine pesticide residues (0.12 ppm) and 3 fortified PCB residues (0.80 ppm) from flounder, bluefish, and shad samples, which contained 0.8,5.4, and 22.6% fat, respectively. For the 3 types of fish, recoveries of 23 of 24 fortified organochlorine pesticide residues ranged from 55 to 129%, and recoveries of 3 fortified PCB residues ranged from 55 to 104%. There were no significant differences in recovery based on fish species and/or fat content for the majority of residues studied. This SPE method and the official AOAC method yielded comparable results for fish containing incurred organochlorine residues.

scholarly journals Simultaneous Determination of Imazalil and Its Major Metabolite in Citrus Fruit by Solid-Phase Extraction and Capillary Gas Chromatography with Electron Capture Detection

2001 ◽  
Vol 84 (2) ◽  
pp. 546-550 ◽  
Author(s):  
Hisashi Matsumoto
Keyword(s):  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Simultaneous Determination ◽  
Capillary Gas Chromatography ◽  
Solid Phase ◽  
Citrus Fruit ◽  
Electron Capture Detection ◽  
Phase Extraction ◽  
Spe Method

Abstract A method was developed for the simultaneous determination of imazalil and its major metabolite, R 14821, in citrus fruit. This method (designated the SPE method) is based on solid-phase extraction (SPE) and capillary gas chromatography (GC) with electron-capture detection (ECD). The SPE method is highly sensitive for both compounds (limit of detection for each: 0.001 μg/g) and is less time consuming than the previously reported method based on repeated liquid–liquid partitioning and GC–ECD. Recoveries for 3 levels of fortification (0.02, 0.2, and 2.5 μg/g) from satsuma mandarins ranged from 94.3 to 96.5% for imazalil and from 93.9 to 96.3% for R 14821, with coefficients of variation (CVs) ranging from 3.1 to 6.3% for imazalil and from 4.5 to 5.6% for R 14821. Average residual levels found in grapefruit, oranges, and lemons by the SPE method and the previously reported method, and the corresponding CVs, were similar.

scholarly journals Determination of dimethoate, 2,4-dichlorophenoxy acetic acid, mecoprop and linuron pesticides in environmental waters in Republic of Macedonia by high performance liquid chromatography

2008 ◽  
Vol 27 (1) ◽  
pp. 25 ◽  
Author(s):  
Aleksandra Nestorovska-Krsteska ◽  
Meri Mirčeska ◽  
Jean-Jacques Aaron ◽  
Zoran Zdravkovski
Keyword(s):  
Acetic Acid ◽  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Sampling Period ◽  
Phase Extraction ◽  
Environmental Waters ◽  
Spe Method ◽  
Dichlorophenoxy Acetic Acid

An HPLC-UVDAD method for determination of dimethoate, 2,4-dichlorophenoxy acetic acid (2,4-D), mecoprop (MCPP) and linuron in environmental waters was developed. The water samples were concentrated and extracted by a solid phase extraction (SPE) method on Bond Elut PPL cartridges. After extraction the investigated compounds were separated on Stability RP Pesticides chromatographic column using mobile phase composed of acetonitrile- water-acetic acid in volume fractions of 39:59:2 and flow rate of 0.7 mL/min. Ultraviolet absorption detection was carried out for dimethoate, 2,4-D and MCPP at 229 nm, and for linuron at 249 nm. Recoveries made from 500 mL of drinking waters using solid phase extraction ranged between 64.3–92.1 %. The method was applied to environmental waters in Macedonia that receive runoffs from agriculture lands. The levels of pesticides under study ranged between 0.31 μg/L and 7.05 μg/L, depending on the compound and sampling period.

Validation of the Pseudo Imprinted Microspheres for Solid-Phase Extraction of Acyclovir from Swine Tissue

2011 ◽  
Vol 393-395 ◽  
pp. 1591-1594
Author(s):  
Feng Xia Qiao ◽  
Hong Yuan Yan
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Suspension Polymerization ◽  
Aqueous Suspension ◽  
Selective Extraction ◽  
Phase Extraction ◽  
Matrix Interferences ◽  
The Matrix ◽  
Extraction Volume ◽  
Swine Tissue

The novel pseudo imprinted microspheres were synthesized by aqueous suspension polymerization using theophylline as the template and employed as a special sorbent of solid-phase extraction for selective extraction of acyclovir from swine tissue. The pseudo imprinted microspheres revealed high affinity and selectivity to acyclovir, and the matrix interferences could be efficiently eliminated, which make the extract of solid-phase extraction clean enough for HPLC analysis. The parameters that affect the extraction efficiency of solid-phase extraction were investigated, including solvent of extraction, volume of loading sample, washing and elution solvent, etc. Good linearity was obtained in a range of 0.05~15 μg/mL with correlation coefficient (r2) of 0.9991. The recoveries at three spiked levels were ranged from 91.4% to101.0% with RSD less than of 5.0%.

scholarly journals Development of a Solid-Phase Extraction Method for Determination of Pheophorbide a and Pyropheophorbide a in Health Foods by Liquid Chromatography

2004 ◽  
Vol 87 (4) ◽  
pp. 937-942 ◽  
Author(s):  
Harumi Oshima ◽  
Eiji Ueno ◽  
Isao Saito ◽  
Hiroshi Matsumoto
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Reversed Phase ◽  
Official Method ◽  
Phase Extraction ◽  
Pheophorbide A ◽  
Significant Difference ◽  
Spe Method

Abstract A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1–102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 μg/g and from <1 to 24 μg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid–liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.

scholarly journals Syringe-Cartridge Solid-Phase Extraction Method for Patulin in Apple Juice

2003 ◽  
Vol 86 (6) ◽  
pp. 1160-1163 ◽  
Author(s):  
Thomas A Eisele ◽  
Midori Z Gibson
Keyword(s):  
Solid Phase Extraction ◽  
Apple Juice ◽  
Solid Phase ◽  
Potassium Phosphate ◽  
Test Sample ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Phase Liquid ◽  
Spe Method

Abstract A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 μg/kg in an industrial quality assurance laboratory environment.

scholarly journals Determination of Organic Acids in Salicornia herbacea by Solid-phase Extraction Combined with Liquid Chromatography

2013 ◽  
Vol 8 (2) ◽  
pp. 1934578X1300800
Author(s):  
Damian Han ◽  
Minglei Tian ◽  
Dong Wha Park ◽  
Kyung Ho Row
Keyword(s):  
Solid Phase Extraction ◽  
Ferulic Acid ◽  
Caffeic Acid ◽  
Solid Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Trifluoracetic Acid ◽  
Spe Method ◽  
Salicornia Herbacea

A solid-phase extraction (SPE) method for the determination of procatechuic acid, ferulic acid and caffeic acid in Salicornia herbacea L. (Hamcho) has been developed. The optimal conditions were obtained by using a C18 SPE cartridge. By using ethanol and acetonitrile /water/ trifluoracetic acid as washing and eluting solvents, most interfering compounds originating from the hamcho matrix were eliminated. The extracts were sufficiently clean to be directly injected into the HPLC for further chromatographic analysis. Good linearity was obtained from 0.1 to 200 μg/mL (r > 0.999) for procatechuic acid, 0.2 to 400 μg/mL (r > 0.999) for caffeic acid and 0.3 to 600 μg/mL (r > 0.999) for ferulic acid, with the relative standard deviations being less than 3.6%. The mean recoveries of procatechuic acid, ferulic acid and caffeic acid from hamcho were more than 79.2% and the detection limit (S/N = 3:1) was 0.02 μg/mL for procatechuic acid, 0.01 μg/mL for caffeic acid and 0.04 μg/mL for ferulic acid. This method is a viable alternative to the existing HPLC methods for analyzing the content of procatechuic acid, ferulic acid and caffeic acid in hamcho.

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