scholarly journals Toxicity of primulic acid 1 against a daphnid species Simocephalus expinosus s.l.

2021 ◽  
Vol 0 (0) ◽  
Author(s):  
M. Lukáč ◽  
M. Pisárčik ◽  
R. Horáková ◽  
M. Bajcura ◽  
B. Horváth ◽  
...  

Abstract Primulic acid 1 is the main saponin present in Primula elatior. The present study describes the isolation of this amphiphilic compound from primula root. It was performed by ultrasonic maceration, reverse-phase column chromatography and crystallization. Investigations of its physicochemical property are represented by the determination of critical micelle concentration (cmc). The cmc value of the amphiphile was 9.4 × 10−5 mol·dm−3. The evaluation of environmental toxicity was performed on a daphnid species Simpocephalus expinosus s.l., which was very sensitive to primulic acids 1. The results from acute immobilisation test show that the tested compound has half maximal effective concentration after 24 hours (EC50-24 h) equal to 6.9 mg·l−1. Saponin can be classified as a toxic compound for aquatic organisms.

1987 ◽  
Vol 70 (6) ◽  
pp. 964-966
Author(s):  
Dorothy R Heidemann ◽  
Edward S Schulenberg ◽  
William H Smith

Abstract Buffered solid dosage forms containing aspirin, magnesium hydroxide, and aluminum hydroxide are blended with acidic ethanol to extract the aspirin and salicylic acid rapidly. The resulting preparation is then immediately injected onto a 4.6 mm x 3 cm 5 (im reverse-phase column. Aspirin and free salicylic acid are determined simultaneously. The run time is <2 min. The total time from the initiation of sample extraction to completion of the separation is <5 min.


1982 ◽  
Vol 30 (6) ◽  
pp. 2287-2290 ◽  
Author(s):  
Hisanobu Yoshida ◽  
Ikue Morita ◽  
Tsutomu Masujima ◽  
Hideo Imai

1984 ◽  
Vol 67 (6) ◽  
pp. 1058-1061
Author(s):  
Harvey L Kramer

Abstract A liquid chromatographic (LC) method is described for the determination of sodium fluoroacetate in meat baits and formulations. Baits were extracted with water, ultrafiltered, partitioned into butanone, back-partitioned into dilute base, and diluted with acetonitrile. Aqueous formulations of 1080 were diluted with acetonitrile. The solutions were esterified with p-bromophenacyl bromide, using crown ether catalysis, and chromatographed on a 10 μm reverse phase column. Ultraviolet absorbance was monitored at 260 nm. Samples spiked to contain 1 mg and 10 mg 1080/100 g meat gave recoveries of 84.0-103.4%.


1987 ◽  
Vol 70 (3) ◽  
pp. 538-540
Author(s):  
Ugo R Cieri

Abstract A method is presented for the liquid chromatographic (LC) determination of ergotamine tartrate in tablets that is applicable even in the presence of other ingredients such as phenobarbital, belladonna alkaloids, and caffeine. The sample is transferred to a volumetric flask, a small volume of formic acid is added to dissolve and stabilize the ergotamine, and the solution is diluted to volume with methanol. The solution is mixed and filtered through paper. The LC system consists of a Rheodyne injector fitted with a 20 μL loop and a C,18 reverse phase column; the mobile phase is acetonitrile-water-triethylamine (700 + 300 + 0.5). Ergotamine tartrate is determined fluorometrically at an excitation wavelength of 250 nm and an emission wavelength of 430 nm. Recovery studies were conducted at the 0.3 and 1.0 mg levels. Average recoveries were 99.6 and 100.8%, respectively; relative standard deviations (RSDs) were 1.08 and 2.21%, respectively. Some commercial preparations containing ergotamine tartrate in combination with other ingredients were also analyzed. The RSDs for 5 determinations of each of 2 ground composites were 0.09 and 0.34%.


1986 ◽  
Vol 69 (1) ◽  
pp. 35-36
Author(s):  
Mary W Trucksess ◽  
Michael T Flood ◽  
Samuel W Page

Abstract The thin layer chromatographic (TLC) method of Trucksess et al. (J. Assoc. Off. Anal. Chem. (1984) 67, 40-43) was modified for the determination of deoxynivalenol (DON) in high-sugar breakfast cereals, corn syrup, and beer. Celite was added to the substrate before extraction with acetonitrile-water (84 + 16). After filtration through an aluminacharcoal-Celite (0.5 + 0.7 + 0.3) column, the filtrate was evaporated to dryness and redissolved in water, which was passed through an octylsilyl reverse phase column. DON was eluted with anhydrous ethyl ether. The residue remaining after the eluate was evaporated to dryness was dissolved in CHCl3-acetonitrile (4 + 1) and chromatographed on AlCVimpregnated silica gel TLC plates. The blue fluorescent DON spot was quantitated fluorodensitometrically after the TLC plate was heated at 120°C for 7 min. Recoveries of DON added to breakfast cereals at 100, 200, and 400 ng/g levels and to syrup and beer at 50, 100, and 200 ng/g levels averaged 86%. The limit of determination in these products was about 50 ng/g.


1988 ◽  
Vol 71 (6) ◽  
pp. 1106-1109
Author(s):  
Theo J Spierenburg ◽  
Henk Van Lenthe ◽  
Gertjan De Graaf ◽  
Lowie P Jager

Abstract A liquid chromatographic method for the determination of olaquindox in both medicated feeds and porcine gastrointestinal tract is described. Samples are extracted with water and cleaned on a disposable reverse-phase column. The eluate is chromatographed on a reverse-phase column under isocratic conditions. Olaquindox is detected by UV absorption at 260 nm. The minimum amount detected by this method was 0.075 ng. The corresponding minimum detectable concentration in a 1 g sample was 0.3 mg/kg. The detector response was linear within the interval of 0-500 ng. Mean recovery of olaquindox in spiked gastrointestinal samples was 89 ± 5% (mean ± standard deviation, n = 43). Concentration profiles of olaquindox in the gastrointestinal tract of pigs fed medicated feed were used to evaluate the preventive potency against Treponema hyodysenteriae. The presence of some N-O reduced metabolites of olaquindox in the gastrointestinal tract was assessed


1985 ◽  
Vol 68 (6) ◽  
pp. 1131-1133
Author(s):  
Jacobus J L Hoogenboom ◽  
Colin G Rammell

Abstract A chloroform extract of stomach contents at basic pH is concentrated and then extracted with 0.1M phosphoric acid. The acid extract is chromatographed on a 10 cm reverse phase column, using 0.005M phosphate buffer (pH 3.0)-acetonitrile-tetrahydrofuran (750 + 135 + 115) containing 0.01M octanesulfonic acid at a flow rate of 1.0 raL/ min for elution. Strychnine eluted in 7.3 min. Recoveries from spiked stomach contents averaged 92%. The method can be used without modification for other alkaloids.


1990 ◽  
Vol 73 (6) ◽  
pp. 893-895 ◽  
Author(s):  
Ajay G Patel ◽  
Ramanbhai B Patel ◽  
Mukeshbhai R Patel

Abstract A liquid chromatographic (LC) method has been developed for determination of clobetasone-17-butyrate In ointment using clobetasone propionate as an internal standard. Separation was carried out on a C18 reverse-phase column using water-methanol as a mobile phase. Methylparaben and propylparaben (both sodium salt) used as preservatives did not Interfere with separation. Compounds are detected photometrically at 235 nm. Mean assay results for 0.05% commercial ointments were 100.36% (n = 5). Mean recovery of clobetasone-17-butyrate added to commercial ointment was 99.89%.


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