HPLC chromatograms sample

Figure 2.11 (a) HPLC chromatogram obtained for a sample of drinking water spiked with... 

FIGURE 25 HPLC chromatograms of polymer samples hydrolyzed to cleave all ortho ester bonds. Samples were prepared at either 130, 145, or leO C. Polymer prepared from 3,9-bis(ethylidene-2,4,8,10-tetraoxaspiro)5,5]undecane) and a 25 75 mole ratio of trans-cyclohexane dimethanol and 1,6-hexanediol and contained 3 wt% phthalic anhydride and 7.5 wt% cyclobenzaprine hydrochloride (CBP). 

FIGURE 25.3 (a) The HPLC chromatogram of the extract obtained from a yellow-pigmented sample of... 

FIGURE 1.43 Representative HPLC chromatograms of vitamin D metabolites.162 (A) late-eluting peaks (B) calibrator in extracted serum (C) sample from patient with low 25(OH)D3 treated with vitamin D2 (D) sample from patient with high concentrations of 25(OH)D3. Int. Std. = internal standard mAU = milliabsorbance units. (Reproduced with permission from the American Association for Clinical Chemistry.)... 

Figure 11 (a) and (b) shows the HPLC chromatograms of penicillins in production sample and standard solution respectively ... 

Fig. 2.18. HPLC chromatogram of carotenoids in an authentic sample of orange juice I Sudan I, II lutein, III zeaxanthin, IV /J-cryploxanlhin. V a-carotene, VI / -carotene. For chromatographic conditions see text. Reprinted with permission from A. M. Pupin et al. [42].

Fig. 2.72. Examples of HPLC chromatograms (a) calibration standards (b) commercial orange fruit juice sample (c) hand-sqeezed grapefruit juice sample. Peaks (d) diosmin (h) hesperidin (n) naringin (IS) rhoifolin (internal standard). Reprinted with permission from. F. I. Kanaze et al. [190],...

Fig. 2.158. HPLC chromatogram of a sample of the superficial layer of the pink astragalos. Reprinted with permission from M. P. Colombini et al. [330].

Fig. 3.25. Composite overlay of HPLC chromatograms of the control reagents blank standard containing 5 ng LGV and 0.5 ng GC 0.5 g equivalent of control catfish sample 1 h post-dosing sample 7 h post-dosing sample 15 days post-dosing sample and 79 days post-dosing sample. Samples are mean of n = 5. Reprinted with permission from H. C. Thompson Jr et al. [104],...

Fig. 3.72. (a) Standard HPLC chromatogram. (1) Benzidine, (2) o-toluidine, (3) 4-chloroaniline, (4) 3,3-dimethoxybenzidine, (5) 3,3-dimethylbenzidine, (6) 4-aminobiphenyl (7) 3,3-dichloroben-zidine. Detection wavelength 280 nm amino concentration approximately 50 pg/ml. HPLC conditions are described in the text, (b) Chromatogram of a genuine leather sample treated with the MAE procedure. Reprinted with permission from C. S. Eskilsson et al. [140]. 

Fig. 3.132. HPLC chromatograms of (a) Reactive brown 23 (420 nm detection), (b) Reactive red 2 (Aldrich, 538 nm), and (c) Reactive orange 4 (490 nm) during hydrolysis. Dyes were dissolved at 10 mg/ml in 50 mM Na2C03 pH 10.5. Samples were removed for HPLC analysis at regular time intervals (t). Reactive brown was diluted to 2 mg/ml and injected Reactive red 2 and Reactive orange...

The precipitate was then analyzed using high performance liqnid chromatography (HPLC) to reaffirm the results as characterized by the IR analysis. The precipitate was collected and dissolved in an acetone solntion with water (1 2 v/v) acting as the solvent before the analysis was done. Finally, the 1.0 ppm concentrated sample was injected into a HPLC machine. The chromatogram shows a peak at the retention time (Rj) which is almost the same as the retention time of standard vanillin with the same concentration. Figure 9.4 presents the HPLC chromatograms of the vanillin sample and the standard vanillin. 

Both WSV and FSV methods were rapid, with extraction and analysis completed in an honr. A single tablet was used to minimize sample volume and solvent nse. This is more acceptable for OTC prodncts. Further details and data were published elsewhere. Table 4 shows assay data on precision and recovery and Figure 7 shows HPLC chromatograms of WSV in standard solution and in multivitamin extracts. 

In HPLC, a sample is separated into its components based on the interaction and partitioning of the different components of the sample between the liquid mobile phase and the stationary phase. In reversed phase HPLC, water is the primary solvent and a variety of organic solvents and modifiers are employed to change the selectivity of the separation. For ionizable components pH can play an important role in the separation. In addition, column temperature can effect the separation of some compounds. Quantitation of the interested components is achieved via comparison with an internal or external reference standard. Other standardization methods (normalization or 100% standardization) are of less importance in pharmaceutical quality control. External standards are analyzed on separate chromatograms from that of the sample while internal standards are added to the sample and thus appear on the same chromatogram. 

FIGURE I Typical fast HPLC chromatograms for a set of three dissolution samples at three time points. 

Understandably, the impurity profiles of the same drug substance produced by different S3mthetic routes will differ qualitatively and quantitatively. This is commonly observed when a drug substance is provided by different suppliers. For example, the HPLC chromatograms from samples of fluoxetine hydrochloride obtained from four different suppliers show the differences in the impurities produced by the presumably different synthetic routes (Figure 1.1) [7]. Supplier A is the innovator company. Supplier B is in Italy, and Suppliers C and D are in India. 

Figure 1.1 HPLC chromatograms of samples of fluoxetine hydrochloride from four different suppliers (A-D). Reproduced from [7], Reproduced by permission from the publisher and authors. (Column 250 X 4.6 mm i.d. 5 pm Zorbax SB-C8 mobile-phase gradient acetonitrile water triflu-oroacetic 20 80 0.07 for 5 min, to 85 15 0.07 over 25 min, maintain at 85 15 0.07 for 5 min, return to initial conditions over 5 min, re-equilibrate for 10 min flow rate 1 mEmin injection 10 pi of 10 mg/ml solution in the initial mobile phase detector UV 260 nm.)...

Figure 5.4 Reversed-phase HPLC chromatogram of a sample of the complex alkaloid cryp-tospirolepine (11) that had been stored in de-DMSO in a sealed NMR tube for a period of 10 years. None of the starting alkaloid remains there are a total of 26 components observed in the chromatogram, the two major peaks at 16.591 and 18.123 min retention times constituting >45% of the degraded sample.

Figure 6.2 A comparison of HPLC separation methods, (a) HPLC of a-chaconine and a-solanine in the flesh and the peel of one variety of potato. Conditions column, Inertsil NH2 (5 xm, 4.0 X 250 mm) mobile phase, acetonitile/20 mM KH2PO4 (80 20, v/v) flow rate, I.OmL/min column temperature, 20°C UV detector, 208 nm sample size, 20 (xL. (b) HPLC chromatogram of approximately 1 xg of each of potato glycoalkaloids and their hydrolysis products 1, solasonine (internal standard) 2, a-solanine 3, a-chaconine 4, P2-solanine 5, pi-chaconine 6, (32-chaconine 7, y-solanine 8, y-chaconine. Conditions column. Resolve Cl 8 (5 (xm, 3.9 x 300 mm) mobile phase, 35% acetonitrile/100 mM ammonium phosphate (monobasic) at pH 3 flowrate, I.OmL/min column temperature, ambient UV detector, 200 nm sample size, (c) HPLC chromatogram of the aglycones solanidine and solasodine. Conditions column Supelcosil C18-DB (3 (xm, 4.6x150 mm) mobile phase, 60% acetonitrile/10 mM ammonium phosphate pH 2.5 flowrate, 1.0 mL/min column temperature, ambient UV detector, 200 nm.

Fig. 5.4.9 HPLC chromatogram of the derivatised free BA fraction obtained from a human serum sample from a patient with primary biliary cirrhosis (PBC) before (a) and after (b) treatment with ampicillin. 1 CDCA, 2 DCA, 3 lauric acid (internal standard), 4 LCA. R peak represents the reagent peak. (Reprinted from [20])...

Figure 1. HPLC chromatograms of an authentic sample (0.255 lAg) of salvinorin A (A), and of representative Salvia divinorum tissue extracts obtained from "Palatable" clone (Bret Blosser) (B), from Cerro Rab6n clone (L. J. Valdes) (C), and from a seed grown plant DS03 (D. J. Siebert) (D). In each case the retention time of the peak representing salvinorin A is indicated. (For chromatographic protocol see Experimental section).

Figure FI. 3.4 shows HPLC chromatograms for anthocyanidins generated from acid hydrolysis of concord grape and strawberry juices. Extraneous peaks may be present because of incomplete hydrolysis, and degradation and polymerization of the labile aglycons even more of a problem. For acylated anthocyanins, higher yields of anthocyanidins will be achieved if the sample is first saponified (see Basic Protocol 3) and then subjected to acid hydrolysis (see Basic Protocol 2).

Figure F1.3.6 HPLC chromatograms of radish anthocyanin extract before (solid line) and after (dashed line) saponification. Peak 1 pelargonidin-3-sophoroside-5-g ucoside Peaks 2, 3, 4, 5 pelargonidin-3-sophoroside-5-glucoside acylated with />coumaric (2), ferrulic (3), p-couniaric and malonic (4), or ferrulic and malonic acid (5), respectively. Note that the saponified sample has only pelargonidin-3-sophoroside-5-glucoside.

Fig. 10 HPLC chromatograms of supercritical fluid extracts of (A) an unfortified wheat sample and (B) a vitamin A-fortified bran-based ready-to-eat breakfast cereal. Column, 5-/rm Altex C8 (octyl) (150 X 4.6-mm ID) mobile phase, acetonitrile/2-propanol/aqueous 25 mM sodium perchlorate (45 45 10), 2.0 ml/min amperometric detection (oxidative mode), glassy carbon electrode, +1.2 V, vs saturated calomel electrode. Peak (1) retinyl palmitate. (Reprinted from Ref. 90, Copyright 1997, with the kind permission of Elsevier Science-NL, Sara Burgerhartstraat 25, 1055 KV Amsterdam, The Netherlands.)...

The use of the HPLC technique with a programmable fluorescence detector was described for FLU analysis (201). This method was compared with on-line microdialysis used as the cleanup step for a chicken liver sample. After the on-line microdialysis sample cleanup, the resultant HPLC chromatograms were free of background interference, enabling the programmable detector to optimize the quantitation of the three analytes in a single run. The limit of quantitation was 1 yug/ml. 

Fig. 2 Reversed-phase HPLC chromatogram of the dansyl derivatives of amines from a sample of spoiled table olives. Peak identities 1, putrescine 2, cadaverine 3, 1,7-diaminoheptane (IS) 4, tyramine. (From Ref. 19.)...

Figure 5.2.3 HPLC chromatogram of a raw tomato peel sample 150 x 4.6 mm C30 column (ProntoSil, 3 p.m, 200 A, Bischoff, Germany), flow rate 1 ml/min, 22 °C, 469 nm, eluent acetone/ water. Gradient steps (1) 3 min with 75/25 (v/v) acetone/water (2) a 24-min gradient to 100% acetone (3) an 18-min hold at 100 % acetone (4) a 2-min gradient back to the initial conditions...

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