Ammonia sample chromatogram

Figure 6. Typical ion chromatogram of an experimental sample containing ammonia and methylamines...

Figure 13.9 Coupled-column RPLC-UV (215 nm) analysis of 100 p.1 of an extract of a spiked soil sample (fenpropimorph, 0.052 mg Kg-1). LC conditions C-l, 5 p.m Hypersil SAS (60 m X 4.6 mm i.d.) C-2, 5 p.m Hypersil ODS (150 m X 4.6 mm i.d.) M-l, acetonitrile-0.5 % ammonia in water (50 50, v/v) M-2, acetonitrile-0.5 % ammonia in water (90 10, v/v) flow-rate, 1 ml min-1 clean-up volume, 5.9 ml transfer volume, 0.45 ml. The dashed line represents the chromatogram obtained when using the two columns connected in series without column switching. Reprinted from Journal of Chromatography A, 703, E. A. Hogendoorn and P. van Zoonen, Coupled-column reversed-phase liquid chromatography in environmental analysis , pp. 149-166, copyright 1995, with permission from Elsevier Science.

Fig. 2.6 Ion chromatograms, ammonia in river water (left) and rainwater (right). Measuring conditions were as follows (river water) sample, 1 ml ...

TLC has also been used for quantitative determinations of the tropane alkaloids. Belladonna alkaloids can be determined by quantitative TLC (Samples of Belladonna are extracted according to the method of Pharm. Helv. V (Swiss Pharmacopeia V). The alkaloids so extracted are then separated on kiesel gel G plates with the solvent acetone-aqueous ammonia (19 1). After development, the chromatograms are dried, sprayed with Dragendorff s reagent and the areas of the spots are measured. 

Beckett and Triggs were interested in the determination of nicotine and its main metabolite cotinine in urine. An acidified urine was extracted with diethyl ether to remove impurities, the urine was made alkaline with sodium hydroxide and the nicotine extracted with diethyl ether. Cotinine was extracted from urine with methylene chloride after basification of the sample with ammonia. On concentration of the solution, the gas chromatography was carried out on a packed column treated with KOH using Carbowax 20 M as stationary phase. A relative recovery of 95-100 % for the two alkaloids was obtained with respect to their internal standard, chlorophentermine for nicotine and lignocaine for cotinine, which were added to the urine at the start of the assay procedure. Typical chromatograms are given in Figure 4. 

Fig. 4.8. Thin-layer chromatogram. Conditions TLC plate spread the mixture of silica gel GF254 (5 g) and 0.5% CMC solution (14 mL) onto the 10 x 20 cm glass plate concentration of standards (Mal-/3-CD, maltose and /S-CD) and sample aqueous solution lOmg/mL spotting amount 10 /rL developer n-propanol ethyl acetate water 25% ammonia = 6 2 5 3 expend twice at 30°C upwardly dry, irradiate at 254 nm UV light develop the color reaction by iodine vapor [ 12].

---