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  • Automated in-tube solid-phase microextraction-liquid chromatography-electrospray ionization mass spectrometry for the determination of ranitidine.

Automated in-tube solid-phase microextraction-liquid chromatography-electrospray ionization mass spectrometry for the determination of ranitidine.

Journal of chromatography. B, Biomedical sciences and applications (1999-10-08)
H Kataoka, H L Lord, J Pawliszyn
ABSTRACT

The technique of automated in-tube solid-phase microextraction (SPME) coupled with liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) was evaluated for the determination of ranitidine. In-tube SPME is an extraction technique for organic compounds in aqueous samples, in which analytes are extracted from the sample directly into an open tubular capillary column by repeated aspirate/dispense steps. In order to optimize the extraction of ranitidine, several in-tube SPME parameters such as capillary column stationary phase, extraction pH and number and volume of aspirate/dispense steps were investigated. The optimum extraction conditions for ranitidine from aqueous samples were 10 aspirate/dispense steps of 30 microliters of sample in 25 mM Tris-HCl (pH 8.5) with an Omegawax 250 capillary column (60 cm x 0.25 mm I.D., 0.25 micron film thickness). The ranitidine extracted on the capillary column was easily desorbed with methanol, and then transported to the Supelcosil LC-CN column with the mobile phase methanol-2-propanol-5 M ammonium acetate (50:50:1). The ranitidine eluted from the column was determined by ESI-MS in selected ion monitoring mode. In-tube SPME followed by LC-ESI-MS was performed automatically using the HP 1100 autosampler. Each analysis required 16 min, and carryover of ranitidine in this system was below 1%. The calibration curve of ranitidine in the range of 5-1000 ng/ml was linear with a correlation coefficient of 0.9997 (n = 24), and a detection limit at a signal-to-noise ratio of three was ca. 1.4 ng/ml. The within-day and between-day variations in ranitidine analysis were 2.5 and 6.2% (n = 5), respectively. This method was also applied for the analyses of tablet and urine samples.

MATERIALS
Product Number
Brand
Product Description

Supelco
SUPELCOSIL LC-NH2-NP HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-NH2-NP Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
Omegawax Capillary GC Column, L × I.D. 15 m × 0.10 mm, df 0.10 μm
Supelco
SUPELCOSIL LC-CN Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-CN HPLC Column, 5 μm particle size, L × I.D. 15 cm × 4.6 mm
Supelco
SUPELCOSIL LC-CN HPLC Column, 5 μm particle size, L × I.D. 25 cm × 4.6 mm
Supelco
SUPELCOSIL LC-CN HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 3 mm
Supelco
Omegawax Capillary GC Column, L × I.D. 30 m × 0.25 mm, df 0.25 μm
Supelco
SUPELCOSIL LC-CN HPLC Column, 3 μm particle size, L × I.D. 7.5 cm × 4.6 mm
Supelco
Omegawax Capillary GC Column, L × I.D. 30 m × 0.32 mm, df 0.25 μm
Supelco
SUPELCOSIL LC-CN Supelguard Cartridge, 5 μm particle size, L × I.D. 2 cm × 4 mm
Supelco
SUPELCOSIL LC-CN HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 3 mm
Supelco
SUPELCOSIL LC-CN HPLC Column, 3 μm particle size, L × I.D. 3.3 cm × 4.6 mm