Erythrocyte porphyrin analysis in the detection of lead poisoning in children: evaluation of four micromethods.

1976 ◽  
Vol 22 (2) ◽  
pp. 161-168 ◽  
Author(s):  
T L Hanna ◽  
D N Dietzler ◽  
C H Smith ◽  
S Gupta ◽  
H S Zarkowsky

Abstract We evaluated four procedures for determination of erythrocyte porphyrin: double extraction with ethyl acetate/acetic acid-HCl, single extraction with ethanol, single extraction with acetone, and direct solubilization with detergent-buffer. The ethyl acetate procedure, when used with two portions of HCl, apparently gives complete recovery of porphyrin and is suitable for reference as a comparison method. The ethanol procedure gives a high and consistent recovery and is technically simpler. The acetone procedure gives low and variable recovery of porphyrin, and the detergent-buffer method is subject to serious hemoglobin interference; neither of these two procedures offers any technical advantage. Stability of samples and methods for standardization were explored. A procedure for expressing results in terms of erythrocyte Zn-protoporphyrin content is given. Because of its stability, coproporphyrin is useful as a daily working standard. The ethyl acetate and ethanol methods are about equally efficient for detecting lead intoxication. Because of its simplicity, the ethanol method seems to be the best for use in screening.

1975 ◽  
Vol 58 (4) ◽  
pp. 754-756 ◽  
Author(s):  
George M Ware

Abstract Patulin is extracted from apple butter samples with ethyl acetate and the extract is cleaned up on a silica gel column, using benzene-ethyl acetate (75+25) as the eluant. High-pressure liquid chromatography, using a 25 cm Zorbax-Sil column, isooctane-ethyl ether-acetic acid (750+250+0.5) as the mobile solvent, and a 254 nm ultraviolet detector, is used for the determinative step. Under these conditions, patulin is eluted before 5-hydroxymethylfurfural, a component of apple butter which interferes with other liquid chromatographic and thin layer chromatographic methods. Recoveries of patulin added at levels of 34.6, 138.4, and 276.8 μg/kg ranged from 89.0 to 112.1%.


Author(s):  
Rajni Singh Khureja ◽  
Dinesh Kumar

Chromatography is a powerful analytical method suitable for the separation and quantitative determination of a considerable number of compounds, even from complicated matrix. Thin Layer Chromatography (TLC) has some advantages such as rapidity, sensitivity, easiness, cheapness and this method does not require complex instrumental equipment. In present study, Quercetin 3 -O -α- d- glucuro pyranoside (miquelianin; QG), quercetin 3-O-α-d glucopyranoside (isoquercitrin), quercetin 3-O-α-d-galactopyranoside (hyperoside) and rutin in ethyl acetate fractions from aerial parts of selected Potentilla species on a HPTLC plates using a mixture consisting of ethyl acetate/methyl ethyl ketone/diisopropyl ether/formic acid (3:10:4:1, v/v/v/v). Rutinosides and quercetin were also eluted using methanol-water-acetic acid (50/44/6, v/v/v) and benzene: pyridine: formic acid (36:9:5). The spot visualization was evaluated under UV light at 254 nm and Ferric chloride reagent.


2020 ◽  
Vol 67 (12) ◽  
pp. 493-498
Author(s):  
Soichiro Takahashi ◽  
Hudagula ◽  
Noriko Minami ◽  
Rina Sato ◽  
Makoto Kawakami ◽  
...  

2006 ◽  
Vol 71 (6) ◽  
pp. 669-676 ◽  
Author(s):  
Mira Cakar ◽  
Gordana Popovic

A simple, accurate and selective high performance thin layer chromatographic method for the determination of saccharin in pharmaceuticals has been developed. The chromatography was performed on silica-gel 60F254 plates with ethyl acetate-carbon tetrachloride-acetic acid (3 + 4 + 0.5 v/v/v) as the mobile phase. The chromatographic zones corresponding to the saccharin spots were scanned in the reflectance/absorbance mode at ?=230 mm. For the standard curves, two series of saccharin sodium salt solutions were prepared: in methanol (solvent 1) and in ethyl acetate-acetic acid (9:1, v/v) mixture (solvent 2). A linear calibration relationship was observed within the concentration range from 300-1200 ng saccharin sodium salt per spot correlation coefficients being 0.998 (solvent 1) and 0.995 (solvent 2). The relationship between the peak area and the amount of saccharin sodium salt was evaluated by linear regression analysis. The limits of detection and quantification of saccharin sodium salt were 35 ng and 110 ng per spot (solvent 1), respectively, and 45 ng and 150 ng per spot (solvent 2) respectively. Mean recovery values of 103.5 % (solvent 1) and 102.3 % (solvent 2), and RSD values of 4.42 % (solvent 1) and 2.53 % (solvent 2) were obtained. The proposed method was applied for saccharin determination in two pharmaceutical preparations, effervescent tablets and a carbomer- based gel.


1976 ◽  
Vol 59 (3) ◽  
pp. 547-551
Author(s):  
Harris H Wisneski

Abstract A method has been developed for the determination of bergapten (5-methoxypsoralen), a known phototoxin, in perfumes, colognes, and toilet waters. The bergapten and other lactonic compounds were first isolated from the sample by a series of extractions. The extract containing the bergapten was diluted to a known volume and an aliquot was spotted on a thin layer chromatographic (TLC) plate coated with silica gel G. After 2-dimensional development with hexane - carbon tetrachloride - tert - butylamine (180 + 12 + 9) and hexane-toluene-ethyl acetate-acetic acid (100+10+15+0.5), the TLC plate was dried and the emitted fluorescence of bergapten was measured, using a spectrophotofluorometer equipped with a TLC accessory and coupled to an automatic digital integrator. The amount of bergapten was determined by comparing its peak area to those of bergapten standards. The average recovery for levels of 0.001, 0.005, and 0.01% bergapten was 88%.


1976 ◽  
Vol 59 (4) ◽  
pp. 770-776 ◽  
Author(s):  
George H Reazin ◽  
Sidney Baldwin ◽  
Harry S Scales ◽  
Harold W Washington ◽  
Arthur A Andreasen

Abstract A study was made to determine which congeners are derived from ethanol during maturation of whisky. Radioactive ethanol-1-14C was added to a barrel of new bourbon whisky and the radioactivity of the major individual congeners was determined during the maturation period. During 56 months of maturation, ethanol was transformed into acetic acid, acetaldehyde, ethyl acetate, and ethanol lignin as indicated by their radioactivity. No radioactivity was found in the solids, fusel oil alcohols, or the aromatic aldehydes derived from ethanol lignin. The chemistry of maturation is discussed.


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