Oleandomycin phosphate

Infra-red Spectrum. Principal peaks at wavenumbers 1111,1052, 1075, 1010, 1162, 1190 (oleandomycin phosphate). 

Dose. Oleandomycin phosphate has been given in doses of 1 to 2 g daily. 

Sample preparation 1 mL Plasma -t- 20 pL of 100 pg/mL oleandomycin phosphate in ethanol + 60 pL saturated potassium carbonate (final pH 10), mix briefly, add 5 mL t-butyl methyl ether, shake in a reciprocating shaker for 15 min, centrifuge at 800 g for 5 min. Remove 4 mL of the upper ether layer and evaporate it to dryness under a stream of nitrogen at room temperature. Wash down tube with 200 pL t-bulyl methyl ether. Evaporate to dr3mess again, take up residue in 125 pL mobile phase, centrifuge 30 s, inject aliquot. 

Internal standard oleandomycin phosphate (4) Limit of detection 250 ng/mL... 

Sample preparation Prewash a 1 mL CIS Bondelut CIS SPE cartridge with 3 mL MeCN and 3 mL water. 1 mL Serum or urine -(- 0.25 mL (0.50 mL for urine) 6-12 p,g/mL oleandomycin phosphate in water, add 1 mL MeCN, vortex 1 min, centrifuge at 1600 g for 5 min, add to 8 mL water, load onto the SPE cartridge, wash with 5 mL water, wash with 5 mL MeCN. water 1 1, suck dry, elute with two 0.5 mL aliquots of MeCN 50 mM pH 6.30 phosphate buffer. Diy under vacuum in a rotary vacuum centrifuge, reconstitute in 20 p,L water, vortex 1 min, add 25 p,L MeCN, vortex 1 min, centrifuge at 1600 g for 1 min, inject 3-5 pL aliquot of upper layer. 

Sample preparation Centrifuge plasma or gastric juice at 1200 g for 5 min. 500 pL Plasma or gastric juice + 500 pL pH 11 phosphate buffer (ionic strength 1=1.0) + 50 pL 100 pM oleandomycin in MeCN + 5 mL hexane 2-butanol 80 20, shake for 15 min, centrifuge at 1200 g for 5 min, freeze in dry ice/acetone. Remove the organic layer and evaporate it to dryness under a stream of nitrogen, reconstitute the residue in 300 pL mobile phase, vortex three times for 1 min, inject a 40 pL aliquot. 

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