scholarly journals Determination of Chlorobiphenyls in Seal Blubber, Marine Sediment, and Fish: Interlaboratory Study

1996 ◽  
Vol 79 (1) ◽  
pp. 83-96 ◽  
Author(s):  
Jacob De Boer ◽  
Jaap Van Der Meer ◽  
Udo A Th Brinkman
Keyword(s):  
Muscle Tissue ◽  
Marine Sediment ◽  
Standard Error ◽  
Principal Component ◽  
Fish Muscle ◽  
Interlaboratory Study ◽  
Lean Fish ◽  
Seal Blubber Oil

Abstract Between 1988 and 1994, the International Councilfor the Exploration of the Sea, the Intergovernmental Oceanographic Commission, and the Oslo and Paris Commissions organized a stepwise interlaboratory study for determination of chlorobiphenyls (CBs) inmarine media. The final parts of this study, in which 53 laboratories from 14 countries participated, focused on long-term precision, cleanup, and extraction. Calibration was controlled continuously by analysis of 10 CBs in an unknownsolution. Participants were requested toanalyze 3 CBs in a certified reference material fish oil (6 times); 10 CBs in cleaned and uncleaned marine sediment and seal blubber extracts; and 10 CBs in seal blubber oil, dried marine sediment, and wet, lean fish muscle tissue. The long-term precision study showed that, compared with earlier exercises in which only duplicate analyses were required, repeatability increased about 1.5-fold compared with reproducibility. The mean standard error for reproducibility of determination of 10 CBs in standard solutions improved from 1.22 to 1.15. The standard error improved from 1.36 to 1.28(without CBs 28 and 31) for seal blubberoil and from 1.36 to 1.22 for dried marine sediment. In seal blubber oil and dried marine sediment, the major CBs 118,138,153, and 180 can now bedetermined by thegroup of participating laboratories with a reproducibility of 1.5 (about 50%). No significant differences were found between results for cleaned-up and un cleaned extracts. No acceptable results could be obtained for determination ofCBs in lean fish muscle tissue. Biplots of principal component analyses are extremely helpful in evaluating the data generated by this type of study.

Matrix Solid Phase Dispersion Isolation and Liquid Chromatographic Determination of Sulfadimethoxine in Catfish (Ictalurus punctatus) Muscle Tissue

1990 ◽  
Vol 73 (6) ◽  
pp. 868-871 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsieh ◽  
Marsha S Malbrou ◽  
Charles R Short ◽  
Steven A Barker
Keyword(s):  
Muscle Tissue ◽  
Ictalurus Punctatus ◽  
Solid Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Fish Muscle ◽  
Tissue Samples ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method for the isolation and liquid chromatographic determination of sulfadimethoxine In catfish (Ictalurus punctatus) muscle tissue Is presented. Blank control and sulf adlmethox- Ine-fortlfled fish muscle tissue samples (0.5 g) were blended with octadecylsllyl (C18,40 /μm, 18% load, endcapped) derivatlzed silica packing material. A column made from the C18/ fish tissue blend was first washed with hexane (8 mL), following which the sulfadimethoxine was eluted with dlchloromethane (8 mL). The eluant contained sulfadimethoxine analyte that was free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodlode array, 270 nm). Standard curves for sulfadimethoxine Isolated from fortified samples were linear (0.999 ± 0.001) with an average relative percentage recovery of 101.1 ± 4.2% for the concentration range (50, 100, 200,400, 800, and 1600 ng/g) examined using sulfamethoxazole as the Internal standard. The interassay variability was 10.7 ± 8.2% with an Intra-assay variability of 2.2%.

Matrix Solid Phase Dispersion Isolation and Liquid Chromatographic Determination of Oxytetracycline in Catfish (Ictalurus punctatus) Muscle Tissue

1990 ◽  
Vol 73 (6) ◽  
pp. 864-867 ◽  
Author(s):  
Austin R Long ◽  
Lily C Hsiesh ◽  
Marsha S Malbrough ◽  
Charles R Short ◽  
Steven A Barker
Keyword(s):  
Muscle Tissue ◽  
Ictalurus Punctatus ◽  
Solid Phase ◽  
Chromatographic Determination ◽  
Fish Muscle ◽  
Butylated Hydroxytoluene ◽  
Tissue Samples ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method for Isolation and liquid chromatographic determination of oxytetracycllne In catfish (Ictalurus punctatus) muscle tissue Is presented. Blank control and oxytetracycllne- fortlfied fish muscle tissue samples (0.5 g) were blended with octadecylsilyl (C18, 40 μm, 18% load, endcapped) derlvatized silica packing material (2 g) containing 0.05 g each of oxalic acid and disodlum ethylenedlamlnetetraacetate. A column made from the C18/fish tissue matrix was first washed with hexane (8 mL), following which the oxytetracycllne was eluted with acetonltrile-methanol (1 + 1, v/v) containing 0.06% w/v each of butylated hydroxyanlsole and butylated hydroxytoluene. The eluate contained oxytetracycllne analyte that was free from Interfering compounds when analyzed by liquid chromatography with UV detection (photodlode array set at 365 nm). Standard curves for oxytetracycllne Isolated from fortified samples were linear (0.998 ± 0.002) with an average absolute percentage recovery of 80.9 ± 6.6% for the concentration range (50,100,200, 400, 800, 1600, and 3200 ng/g) examined. The Interassay variability was 11.3 ± 5.2% with an Intra-assay variability of 1.1%.

Determination of Chlorobiphenyls in Cleaned-Up Seal Blubber and Marine Sediment Extracts: Interlaboratory Study

1994 ◽  
Vol 77 (6) ◽  
pp. 1411-1421 ◽  
Author(s):  
Jacob De Boer ◽  
Jaap Van Der Meer ◽  
Lars Reutergårdh ◽  
John A Calder
Keyword(s):  
Marine Sediment ◽  
Interlaboratory Study ◽  
Standard Errors ◽  
Sediment Extract ◽  
Calibration Solution ◽  
Standard Solution ◽  
Study Participants ◽  
Instrument Optimization ◽  
Intergovernmental Oceanographic Commission

Abstract An interlaboratory study on the determination of individual chlorobiphenyl congeners (CBs) in cleaned-up seal blubber and marine sediment extracts was organized by the International Council for Exploration of the Sea, the Intergovernmental Oceanographic Commission, and the Oslo and Paris Commissions, as the second part of a stepwise-designed interlaboratory study on the determination of CBs in marine media. Fifty-eight laboratories from 16 countries participated in this exercise, which involved the determination of 10 CBs in a standard solution, a cleaned-up seal blubber extract, and a cleaned-up marine sediment extract. Suggestions were given for instrument optimization. Standard errors of 1.16–1.17 for the standard solution, 1.20–1.33 for the seal blubber extract, and 1.31–1.56 for the sediment extract were obtained for CBs 52,101,118,138,153, and 180 by all laboratories with the exception of the laboratories giving consistently outlying results. The results for CBs 28,31,105, and 156 showed larger standard deviations. The 2 major difficulties for participants in this exercise were correct preparation of a calibration solution and chromatographic separation. The results of the sediment analysis showed a complete lack of agreement. It is recommended that, prior to the organization of the third part of this study, participants should install gas chromatographic columns with minimum lengths of 50 m and maximum internal diameters of 0.25 mm and should prepare calibration solutions from solids of known purity.

scholarly journals Characterization of the Triacylglycerol Fraction of Italian and Extra-European Hemp Seed Oil

Foods ◽  
2021 ◽  
Vol 10 (5) ◽  
pp. 916
Author(s):  
Carmela Tringaniello ◽  
Lina Cossignani ◽  
Francesca Blasi
Keyword(s):  
Seed Oil ◽  
Principal Component ◽  
Stereospecific Analysis ◽  
Hemp Seed ◽  
Fa Composition ◽  
Chemical Descriptors ◽  
Triacylglycerol Fraction

Hemp seed oil (HSO) has received considerable attention for its health properties, especially due to unsaturated fatty acid (UFA) content. In this work, the triacylglycerol (TAG) fraction of Italian and Extra-European HSO was characterized by applying an enzymatic approach, based on the use of pancreatic lipase and sn-1,2-diacylglycerol kinase. This procedure allows determination of the intrapositional FA% composition of TAG. The results of the stereospecific analysis are useful for deepening knowledge on HSO nutritional aspects. The high percentage of UFA (88.3–89.9%), in particular essential FA (74.4–85.9%), of HSO samples in sn-2 position is important for long-term health effects, but also to enhance the use of this oil as a functional ingredient in food, cosmetic and nutraceutical fields. Furthermore, the results of total and intrapositional FA % compositions, subjected to principal component analysis, were able to differentiate HSO Italian samples from Extra-European ones. Based on the obtained results, it can be stated that the stereospecific analysis represents a potent analytical tool providing the fingerprint of TAG fraction, useful to highlight possible chemical descriptors for HSO authenticity and traceability purposes.

scholarly journals Optimization of an acid digestion procedure for the determination of Hg, As, Sb, Pb and Cd in fish muscle tissue

MethodsX ◽  
2017 ◽  
Vol 4 ◽  
pp. 513-523 ◽  
Author(s):  
Elisabeth Mohammed ◽  
Terry Mohammed ◽  
Azad Mohammed
Keyword(s):  
Muscle Tissue ◽  
Fish Muscle ◽  
Acid Digestion ◽  
Digestion Procedure
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