SCREENING FOR DRUGS IN SERUM AND URINE BY LC / ESI / CID-MS AND MS / MS WITH LIBRARY SEARCHING
A mass spectra library using in-source collision induced dissociation (ESI/CID) as well as a MS/MS library with product ion spectra of ca. 500 drugs have been developed with a triple-quadrupole ionspray mass spectrometer. For the ESI/CID MS library single quadrupole mode and for the MS/MS library triple-quadrupole mode were used. The libraries have been used for general-unknown screening and for identification of drugs and metabolites in serum and urine.
Extraction of benzoylecgonine (cocaine metabolite) and opiates (codeine and morphine) from urine samples using the Zymark RapidTrace.
The Zymark RapidTrace automated solid-phase extraction system has been evaluated for use in the urine drug-testing laboratory. Methods for cocaine metabolite (benzoylecgonine) and opiates (codeine and morphine) are described and evaluated. The linearity, precision, accuracy, recovery, and carryover statistics of these analytical protocols are presented. The advantages of extraction using the RapidTrace instead of solid-phase extraction with the manual vacuum manifold or liquid-liquid extraction methods are described.
HPLC determination of chlorhexidine gluconate and p-chloroaniline in topical ointment.
A novel fast isocratic reversed-phase HPLC method for simultaneous determination of chlorhexidine and its degradation product p-chloroaniline was developed. Zorbax SB Phenyl column (75 mm x 4.6 mm, 3.5 microm) was used for the separation. Mobile phase composed of acetonitrile and buffer solution of 0.08 M sodium phosphate monobasic containing 5 ml of triethylamine (0.5%) and adjust with 85% phosphoric acid to pH 3.0 in ratio 35:65 (v/v) pumped isocratically at flow rate 0.6 ml min(-1) was used. UV detection was performed at 239 nm, the total analysis time was about 10 min. The method is suitable for practical routine analysis of topical ointment in the quality control laboratory.