scholarly journals Micellar Liquid Chromatographic Determination of Carbaryl and 1-Naphthol in Water, Soil, and Vegetables

2012 ◽  
Vol 2012 ◽  
pp. 1-7 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Maria Rambla-Alegre ◽  
Abhilasha Durgbanshi ◽  
Devasish Bose ◽  
Sandeep K. Mourya ◽  
...  

A liquid chromatographic procedure has been developed for the determination of carbaryl, a phenyl-N-methylcarbamate, and its main metabolite 1-naphthol, using a C18 column (250’mm’ × ’4.6’mm) with a micellar mobile phase and fluorescence detection at maximum excitation/emission wavelengths of 225/333’nm, respectively. In the optimization step, surfactants sodium dodecyl sulphate (SDS), Brij-35 andN-cetylpyridinium chloride monohydrate, and organic solvents propanol, butanol, and pentanol were considered. The selected mobile phase was 0.15’M SDS-6% (v/v)-pentanol-0.01’M NaH2PO4buffered at pH 3. Validation studies, according to the ICH Tripartite Guideline, included linearity (r>0.999), limit of detection (5 and 18’ng mL-1, for carbaryl and 1-naphthol, resp.), and limit of quantification (15 and 50’ng mL-1, for carbaryl and 1-naphthol, resp.), with intra- and interday precisions below 1%, and robustness parameters below 3%. The results show that the procedure was adequate for the routine analysis of these two compounds in water, soil, and vegetables samples.

1983 ◽  
Vol 29 (10) ◽  
pp. 1840-1842 ◽  
Author(s):  
J Lehmann ◽  
H L Martin

Abstract We have adapted to erythrocytes a method for the determination of alpha- and gamma-tocopherols in plasma and platelets. Erythrocytes (50 microL) were extracted with methanol containing tocol (internal standard) and pyrogallol. Tocopherols were partitioned into chloroform, washed, and injected in methanol onto a reversed-phase (C18) "high-performance" liquid-chromatographic column. The mobile phase was methanol/water (99/1 by vol) at a flow rate of 2 mL/min and detection was with a "high-performance" spectrophotofluorometer. The limit of detection for either tocopherol is 0.10 microgram/mL of packed cells. Analytical recoveries ranged from 93 to 104%. Some values for tocopherols in human erythrocytes are presented.


Molecules ◽  
2021 ◽  
Vol 26 (13) ◽  
pp. 3791
Author(s):  
Ewelina Patyra ◽  
Krzysztof Kwiatek

Rapid chromatographic procedure for quantification of five sulfonamides in medicated feeds are proposed. Satisfactory separation of sulfonamides from medicated feeds was achieved using a Zorbax Eclipse XDB C18 column (4.6 × 150 mm, 5 µm particle size) with a micellar mobile phase consisting of 0.05 M sodium dodecyl sulphate, 0.02 M phosphate buffer, and 6% propan-2-ol (pH 3). UV quantitation was set at 260 nm. The proposed procedure allows the determination of sulfaguanidine, sulfadiazine, sulfamerazine, sulfamethazine, and sulfamethoxazole in medicated feeds for pigs and poultry. Application of the proposed method to the analysis of five pharmaceuticals gave recoveries between 72.7% to 94.7% and coefficients of variations for repeatability and reproducibility between 2.9% to 9.8% respectively, in the range of 200 to 2000 mg/kg sulfonamides in feeds. Limit of detection and limit of quantification were 32.7–56.3 and 54.8–98.4 mg/kg, respectively, depending on the analyte. The proposed procedure for the quantification of sulfonamides is simple, rapid, sensitive, free from interferences and suitable for the routine control of feeds. In the world literature, we did not find the described method of quantitative determination of sulfonamides in medicated feeds with the use of micellar liquid chromatography.


1986 ◽  
Vol 32 (3) ◽  
pp. 508-510 ◽  
Author(s):  
A Laganà ◽  
G D'Ascenzo ◽  
A Marino ◽  
A M Tarola

Abstract In this precise, accurate, and specific liquid-chromatographic procedure for determining progesterone in serum, the serum is diluted 10-fold with water/methanol (65/35 by vol), and the progesterone is extracted from the sample by passage through a column of graphitized carbon black (Carbopack B, Supelco). After washing the column, we elute the progesterone with chloroform/methanol (90/10 by vol), which is then evaporated. The progesterone is separated on a reversed-phase C18 column with a mobile phase of acetonitrile/water, (46/54 by vol) at a flow rate of 1.6 mL/min. The eluted compound is detected by absorbance at 242 nm. Analytical recoveries for progesterone varied from 96.0 to 97.8%. Within-day and day-to-day precision, determined by analyzing pooled serum, ranged from 3.4 to 6.4%, and 4.1 to 7.9%, respectively. The limit of detection was about 0.2 micrograms/L. Numerous drugs and steroids tested did not interfere. Results correlated (r = 0.997) well with those by radioimmunoassay.


1983 ◽  
Vol 29 (6) ◽  
pp. 1104-1105 ◽  
Author(s):  
B A Robinson ◽  
F N Cornell

Abstract A simple, rapid "high-performance" liquid-chromatographic procedure is presented for the determination of aminoglutethimide in plasma. After precipitation of the protein with acetonitrile, an aliquot of the supernate is injected directly onto a radially compressed, reversed-phase column. The aminoglutethimide is isocratically eluted with a mobile phase of acetonitrile/water/tert-butyl ammonium phosphate. The method is both accurate and precise and has been in routine use in our laboratory for more than 12 months.


1997 ◽  
Vol 80 (4) ◽  
pp. 762-766
Author(s):  
Mythili Nagarajan ◽  
Ted W Waszkuc ◽  
Jidong Sun

Abstract A precise and selective liquid chromatographic procedure for determining inositol hexanicotinate (IHN) in formulated preparations was developed and validated. IHN was dissolved in dimethyl sulfoxide, diluted with acetonitrile, chromatographed on a Nova-Pak C18 column with a mobile phase of water-methanol (40 + 60, v/v), and detected at 262 nm. The correlation coefficient of the calibration curve was 0.9995 over the range 0.050.15 mg/mL. Overall recovery of IHN was >97%. Coefficients of variation for intra- and interday precisions were <2%.


1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).


1974 ◽  
Vol 57 (5) ◽  
pp. 1089-1091
Author(s):  
David O Edlund ◽  
Florido A Filippini ◽  
James K Datson

Abstract A gas-liquid chromatographic procedure used to determine vitamin D2 in multiple vitamin tablets has been modified to make it applicable for analysis of multiple vitamin tablets containing minerals and vitamin E acetate. The procedure modifications involve pre-extraction with ether, solution in an alcoholic sulfuric acid-pyridine mixture, and column chromatographic separation on phosphate-treated alumina. The modified procedure has been statistically evaluated. A 2.2% coefficient of variation and 100.3% average recovery were obtained for the samples evaluated.


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