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Stool porphyrins determined by high pressure liquid chromatography and by fractional hydrochloric acid--ether extraction.

When stool copro- and protoporphyrin were quantitated by spectrophotometry, after fractional hydrochloric acid-ether extraction, up to 30% of the protoporphyrins were recovered in the coproporphyrin extract. In disorders with elevated stool protoporphyrin excretion (e.g. erythropoietic protoporphyria), this method therefore may give falsely elevated coproporphyrin values. When the stool porphyrins were determined by high pressure liquid chromatography there was no carry-over of protoporphyrin to coproporphyrin. The recoveries were 82 and 87%, and the coefficients of variation 5.6 and 3.1% for proto- and coproporphyrin, respectively. Moreover, in specimens containing a more complex mixture of porphyrins, a complete separation of the C2-C8 porphyrins and porphyrin isomers was obtained in a single run. High pressure liquid chromatography should therefore be considered the method of choice to obtain a quantitative profile of stool porphyrins in the routine laboratory.

Chemical Fractionation↗

[Impact of hydrochloric acid and HP-invasion on the cavitary pressure in the duodenal and gastroesophageal region in patients with ulcer].

The goal of the study was to examine the cavitary pressure (P) in the duodenal and gastroesophageal region under the impact of acidification of the duodenum (D) and depending on the hydrochloric acid gastric secretion (HCL) and Helicobacter pylori (HP) infection in patients with ulcer. Endoscopic manometrography performed in 205 patients (with duodenal ulcer, gastric ulcer and chronic gastritis) revealed a considerable (p<0.05) increase in P (mmHg) in the D (9.4 +/- 0.4 vs. 11.8 +/- 1.0) and in the antral region of the stomach (ARS) (9.6 +/- 0.3 vs. 11.4 +/- 0.6), decreased pylorus tone (33.9 +/- 4.6 vs. 17.5 +/- 6.0) and pressure gradients (AP) between the low esophageal sphincter (LES) and D (6.6 +/- 0.4 vs. 3.9 +/- 1.3) in patients with increased basal acid secretion (BAS (BAS > 10 mm/hour vs. BAS < 7 mm/per hour). Acid infusion of 0.1N HCL in 39 patients was accompanied by the increase of P in the D (from 9.7 +/- 1.1 to 13.1 +/- 1.2), ARS (from 8.6 +/- 1.3 to 12.8 +/- 1.4) and tendency to the reduction in the P in the pylorus (from 28.2 +/- 2.5 to 20.6 +/- 3.6) as well as feeling of pain in all patients with active duodenal ulcers. The presence of HP in 47 out of 87 patients as compared to its absence was associated with the increased deltaP in the D-ARS (-0.6 +/- 0.43 vs. 2.1 +/- 1.1) and reduced deltaP in the LES-D (8.3 +/- 1.6 vs. 3.4 +/- 1.5) and deltaP LES-ARS (14.3 +/- 1.3 vs. 9.8 +/- 1.2) as well as more marked esophagitis (0.64 +/- 0.09 vs. 0.38 +/- 0.11 conventional units, p < 0.05). HP and hypersecreation of HCL synergistically or additively increase the antroduodenal tonic tension, promote the LES incompetence and further damage of the esophageal mucous coat.

Abdominal Pain↗

Use of dicyclohexano-18-crown-6 to separate traces of silver(I) from potassium thiocyanate in hydrochloric acid media, and determination of the silver by atomic absorption spectrometry.

Solvent extraction with 0.05 mol L(-1) dicyclohexano-18-crown-6 (DC18C6) in 1,2-dichloroethane, coupled with flame atomic absorption spectrometry (AAS), has been investigated as a new method for separation of trace amounts of silver(I) from 0.05 mol L(-1) potassium thiocyanate in 1.0 mol L(-1) hydrochloric acid media and quantification of the amount of silver present. The method is based on the formation of an extractable ion-association product, [DC18C6.K](+)[Ag(SCN)(2)](-), with a metal-to-crown ether ratio of 1:1 (as derived from slope analysis data). Stripping of the extracted silver(I) in the 1,2-dichloroethane phase was achieved within 5 min by use of 3.0 mol L(-1) potassium thiocyanate. Reducing the concentration of acid in the sample solution to 0.1 mol L(-1) improved the preconcentration factor severalfold. Excellent tolerance of the proposed method to the presence of foreign ions in solution with silver(I) was demonstrated. A detection limit of 13 ng mL(-1) was derived from the mean value of the blank plus three times its standard deviation. The method was used to determine traces of silver(I) after separation from gold(III), platinum(IV), and palladium(II) matrices on the basis of extractability differences with 18-membered crown ethers under specified conditions. The efficiency of the adopted ion-association mechanism for silver(I) extraction was apparent from the average recovery of 96% for spiked standards by use of the back-washing technique. The proposed extraction procedure was applied to the determination of traces of silver(I) in a selection of chemical reagents.

Journal Article↗