Saccharin flow rate

H3PO4 / 40 % acetonitrile at a flow rate of 1 mL/min. was used, and UV detection at 210 nm was used. The method was used for the separation of benzoic acid, methylparaben, ethylparaben, propylparaben, saccharin, sorbic acids, and /7-hydroxybenzoic acid. 

Fig. 1 Chromatograms of standard solutions (A) containing 1 mg/100 ml of each additive and a sample of raspberry jam spiked with acesulfame-K (B). 1—Acesulfame-K 2—benzoic acid 3—sorbic acid 4— saccharin. Conditions Column PhaseSep Cl8 (250 X 4.6-mm ID), mobile phase 8% methanol-phosphate buffer (8 92), flow rate 1 ml/min. Detection UV, 227 nm. (From Ref. 64.)...

A paired-ion, reversed-phase high-performance liquid chromatographic method was developed for the simultaneous determination of sweeteners (dulcin, saccharin-Na, and acesulfame-K), preservatives (sodium dehydroacetate, SA, salicyclic acid, BA, succinic acid, methyl-para-hydroxybenzoic acid, ethyl-para-hydroxybenzoic acid, n-propyl-para-hydroxybenzoic acid, n-butyl-para-hydroxybenzoic acid, and isobutyl-para-hydroxybenzoic acid), and antioxidants (3-tertiary-butyl-4-hydroxyanisole and tertiary-butyl-hydroquinone). A mobile phase of acetonitrile-50 ml aqueous tr-hydroxyisobutyric acid solution (pH 4.5) (2.2 3.4 or 2.4 3.6, v/v) containing 2.5 mM hexadecyltrimethylammonium bromide and a Clg column with a flow rate of 1.0 ml/min and detection at 233 nm were used. This method was found to be very reproducible detection limits ranged from 0.15 to 3.00 p,g. The retention factor (k) of each additive could be affected by the concentrations of hexadecyltrimethylammonium bromide and a-hydroxyisobu-tyric acid and the pH and ratio of mobile phase. The presence of additives in dried roast beef and sugared fruit was determined. The method is suitable for routine analysis of additives in food samples (81). 

FIGURE 13-5. Analysis of caffeine, saccharin, and benzoic acid. Sample (1) saccharin, (2) caffeine, and (3) benzoate. Column /rBondapak C]8 (10 gm) 3.9 ID mm x 150 mm. Flow rate 1.0 mL/min. Mobile phase 20% MeOH/80% 1 M acetic acid, pH = 2.4. (Note Actual separation will depend upon the quality of the mobile phase and column packing.)... 

Fig. 8-43. Determination of saccharin in a nickel/iron plating bath. - Separator column IonPac NS1 (10 pm) eluent 0.002 mol/L TMAOH (pH 12 with NaOH)/acetonitrile (95 5 v/v) flow rate 1 mL/min detection suppressed conductivity injection 50 pL sample (1 50 diluted).

Fig. 8-80. Analysis of acesulfam-K and saccharin in chewing gum. - Separator column IonPac AS4A eluent 0.0028 mol/L Na2C03 flow rate 2 mL/min detection and injection see Fig. 8-79 (taken from [70]).

Figure 10.173 Determination of saccharin in a nickel/iron bath by ion-exclusion chromatography. Separator column Metrosep Organic Acids eluent 0.5 mmol/L H2S04/acetone (85 15 v/v) flow rate 0.5 mL/min detection ...

Figure 10.267 Analysis of acesulfam-K and injection volume see Figure 10.266 peaks (1) saccharin in a chewing gum sample. Separator fumarate, (2) acesulfam-K, and (3) saccharin column lonPac AS4A eluent 2.8 mmol/L (reproduced with permission from Ref. [435]. Na2C03 flow rate 2 mL/min detection and Copyright 1989, Elsevier B.V.).

Fig. 9-187. Gradient elution of anionic components in a cough suppressant. — Separator column lonPacASll eluant NaOH gradient 0.5 mmol/L isocratic for 2.5 min, then linearly to 5 mmol/L in 3.5 min, then to 38 mmol/L in 12 min flow rate 2 mL/min detection suppressed conductivity injection lOjiL of a 1 10 (w/w) diluted sample solute concentrations (1) and (2) unknown, 0.08 mg/L chloride (3), 30 mg/L bromide (4), 80 mg/L benzoate (5), (6) and (7) unknown, 0.2 mg/L sulfate (8), 0.09 mg/L orthophosphate (9), (10) unknown, 130 mg/L citrate (11), and 120 mg/L saccharin (12).

A potentiometric determination of saccharin was proposed by Fatibello-Filho et al. [86]. In this method, saccharin was potentiometrically measured using a silver wire coated with a mercury film as the working electrode. With this, the main difficulty was the presence of a precipitate (mercurous saccharinate) that could adsorb on tube walls and the electrode surface. To avoid these undesirable effects, a relocatable filter unit was placed before the flow-through potentiometric cell and a surfactant was added to the carrier solution (Figure 24.12). The same investigation team reported the construction and analytical evaluation of a tubular ion-selective electrode coated with an ion pair formed between saccharinate anion and toluidine blue O cation incorporated on a poly(vinyl chloride) matrix [87]. This electrode was constructed and adapted in a FIA system. The optimum experimental conditions found were an analytical path of 120 cm, an injection sample volume of 500 pL, a pH of 2.5, a flow rate of 2.3 mL/min, and a tubular electrode length of 2.5 cm. 

Capitan-Vallvey et al. [89] developed a simple, rapid, and inexpensive monoparameter flow-through sensor for the determination of saccharin. The method is based on the transient adsorption of the sweetener on Sephadex G-25 solid phase packed to a height of 20 mm in the flow cell. The optimal transient retention of the synthetic sweetener, in terms of sensitivity and sampling frequency, was obtained when pH 2.75 citric acid-sodium citrate buffer 5 x 10 M was used as a carrier at a flow rate of 1.5 mL/ min. Saccharin was determined by measuring its intrinsic absorbance at 217 nm at its residence time. The method does not need derivatization reactions and utilized a FIA monochannel manifold similar to those reported by the same investigation team as used to determine other artificial sweeteners [73-75]. 

FIGURE 17 Reversed-phase separation of beverage additives on 10-fjim C-18 silica (Partisil-10 ODS-2). Column 4.6 mm x 25 cm, mobile phase 50 50 methanol-water, flow rate 0.6 ml/min., pressure 529 psi, UV detection at 254 nm. Peaks (a) Saccharin, (b) Theobromine, (c) Theophylline, and (d) Caffeine. [Reprinted by permission from Whatman, Inc.]... 

---