scholarly journals Liquid chromatographic determination of glyphosate and aminomethylphosphonic acid residues in rapeseed with MS/MS detection or derivatization/fluorescence detection

2015 ◽  
Vol 13 (1) ◽  
Author(s):  
Piotr Kaczyński ◽  
Bożena Łozowicka

AbstractGlyphosate and AMPA determinations in rapeseed extracts by (a) liquid chromatography with triple quadrupole MS detection (LC-MS/MS), or (b) liquid chromatography with post-column OPA derivatization and fluorescence detection (LC-FLD) were developed. Mean recoveries for glyphosate and AMPA were (a) 88.8–95.0% and 82.1–86.1%, and (b) 70.8–74.1% and 62.4–72.6%. RSD were below (a) 11% and (b) 22%. Correlation coefficients were above 0.997 for both methods. LOD were 0.01 mg kg

1991 ◽  
Vol 74 (2) ◽  
pp. 317-323 ◽  
Author(s):  
Mark E Oppenhuizen ◽  
John E Cowell

Abstract A new method for determination of glyphosate and amlnomethylphosphonlc acid (AMPA) residues In environmental water was collaboratively studied by 6 laboratories. The method Is simpler and shorter than previous methods. A filtered volume of water is evaporated to dryness and the residue Is dissolved In a buffered EDTA solution. Glyphosate and AMPA are determined by liquid chromatography with postcolumn reaction detection. The method was validated over the range 0.50-5000 ppb, although one of the collaborating laboratories could not reliably quantltate below 1.0 ppb. Statistical analysis of the results showed that typical reproducibility relative standard deviations (RSDR) ranged from 11 to 20% for both glyphosate and AMPA, which compares very well with predicted values for this concentration range. Total variability (as measured by sR) Increased with increasing fortification level. The method has been adopted official first action by AOAC.


1976 ◽  
Vol 59 (1) ◽  
pp. 162-164
Author(s):  
Samuel K Reeder

Abstract A method is presented for the quantitative analysis of o-phenylphenol residues in citrus oils, encapsulated flavors, and dried meal. The method utilizes high-speed liquid chromatography for the determination after specific sample preparations for each material. These preparations include hexane extraction of acidified basic extracts or steam distillation and extraction. The limit of the analysis is <1 ppm with an analysis time of <45 min.


1980 ◽  
Vol 63 (1) ◽  
pp. 49-55
Author(s):  
Iwao Okuno ◽  
Dennis L Meeker

Abstract An analytical method is described for the determination of Compound 1080 (sodium fluoroacetate) residues in 1–10 g tissue. Sample extracts of tissues are cleaned up with silica gel, and Compound 1080 (as fluoroacetic acid) is separated by a micro-distillation procedure. The fluoroacetic acid in the distillate is derivatized with pentafluorobenzyl bromide to form pentafluorobenzyl fluoroacetate which is measured by electron capture gas-liquid chromatography. Recoveries of sodium fluoroacetate from fortified tissue samples averaged about 25%. Despite the limited recoveries, results were quite reproducible, and levels as low at 2 ppm were determined in fortified 1 g samples, and 0.2 ppm in 10 g samples. The method is relatively simple and has been used routinely in our laboratory for the analysis of various types of samples such as grain, and tissues from birds, rodents, and larger animals.


1979 ◽  
Vol 62 (1) ◽  
pp. 171-175 ◽  
Author(s):  
Alfred F Haeberer ◽  
Orestes T Chortyk

Abstract A method is presented for the determination of the plant growth regulator maleic hydrazide (MH; l,2-dihydro-3,6-pyridazinedione) in tobacco and tobacco smoke. Residues are converted to the bis(trimethylsilyl) derivative before analysis by gas-liquid chromatography. The method has been applied to cigarettes and condensed smoke and has been used to determine the per cent transfer of MH into cigarette smoke. Free MH residues could be determined directly on the tobacco samples, whereas total MH values were obtainable only after acid hydrolysis. In spite of large MH residues in tobacco, only 0.2% of the MH was transferred into smoke.


1977 ◽  
Vol 60 (6) ◽  
pp. 1307-1309 ◽  
Author(s):  
Hendrik J Bakker

Abstract Total inorganic iodine in milk is determined by conversion to iodobutanone, which is quantitated by gas-liquid chromatography and electron capture detection. As little as 10 μg/L can be determined. The thyroid-active iodine content of milk can be determined rapidly with a relative standard deviation of 1.9%. Average recoveries for added iodide and iodine were 95.5 and 94.6%, respectively.


1974 ◽  
Vol 57 (2) ◽  
pp. 341-342
Author(s):  
Caesar B Garavelli

Abstract A procedure is described for the quantitative determination of 0.020—6.0 mg choline in low and high potency reference multiple vitamin tablets and standard liver preparations. The trimethylamine quantitatively produced in a sealed tube by treatment with aqueous 5 0% alkali is simultaneously extracted with 0.200—0.500 ml of an isobutanol-ethanol (1+1) mixture and determined by gas-liquid chromatography. An average recovery of 100 ± 3 % was obtained.


1986 ◽  
Vol 69 (5) ◽  
pp. 856-859 ◽  
Author(s):  
Sheldon D West ◽  
Edgar W Day

Abstract A residue method is described for determination of the aquatic herbicide fluridone (1-methy1-3-phenyl-5-[3-(trifluoromethyl)phenyl]-4(1H)- pyridinone) and its metabolite (1-methy1-3-(4-hydroxyphenyl)-5-[3- (trifluoromethyl)phenyl]-4(1H)-pyridinone) in fish and crayfish tissues. Both compounds are extracted from tissues with methanol, and the extracts are subjected to acidic hydrolysis to release conjugated forms of fluridone and the metabolite. Sample extracts are purified by liquidliquid partitioning and Florisil Sep-Pak® column chromatography. Both compounds are separated and measured by reverse phase liquid chromatography with UV detection at 313 nm. In the absence of interfering peaks, the method has a detection limit of approximately 0.04 ppm of either compound. Overall, recoveries averaged 96% for fluridone and 78% for the metabolite for all tissue types combined.


1995 ◽  
Vol 78 (3) ◽  
pp. 841-845 ◽  
Author(s):  
Bertil Lindgren ◽  
Tomas Berglöf ◽  
Åsa Ramberg ◽  
Anna Stepdmska ◽  
Malin Åkerblom

Abstract A method is presented for rapid determination of bromide ion in commodities and blood by paired-ion liquid chromatography with electrochemical detection. The method involves extraction of samples with water and filtration. Blood is passed through a Sep-Pak C18 minicolumn. Recoveries are usually close to 100%, with satisfactory precision. The detection limit is 1 mg/kg. The method needs little labor and uses no noxious solvents or reagents.


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