Rapid detection of diuretics by atmospheric pressure chemical ionization (apci) tandem mass spectrometry
| dc.contributor.author | Muhamad Noh, Hayati | |
| dc.date.accessioned | 2015-07-30T02:27:33Z | |
| dc.date.available | 2015-07-30T02:27:33Z | |
| dc.date.issued | 2003 | |
| dc.description.abstract | Diuretics are banned by the International Olympic Committee (IOC) in sport. The IOC requires mass spectra of at least three diagnostic ions to confirm a positive urine. The cmTent detection method by gas chromatography-mass spectrometry (GC-MS) utilizes derivatization and sample clean-up procedure, which in most instances is a timeĀ· consuming step. The recent development of liquid chromatography (LC) tandem mass spectrometry has demonstrated the capability of detecting a number of drugs; however . the sample clean-up procedure applied to the urine samples is still a time consuming step. A simplified sample preparation followed by detection using LC tandem mass spectrometry was investigated in this study. Atmospheric pressure chemical ionization (APCI) was selected for detection using selected reaction monitoring (SRM) in negative ion mode. The mobile phase containing acetonitrile and 0.05 M ammonium acetate with 0.1% triethylamine (TEA), adjust~d to pH 6.6 established constant ionization conditions for all compounds. Fast gradient elution was accomplished with five minutes run time and a total of eight minutes of analysis cycle time and the diuretics were well separated by their masses. The divert valve on the instrument assist in preventing premature contamination from the early elution. The quadrupole mass analyzer ,parameters including scan speed, resolution, multiplier gain and tube lens were further optimized. Throughout the method validation period, diuretics were detected at the limit of detection of 0.1 ~tg/mL as set by the IOC. All diuretics were also detected by selected ion monitoring (SIM) at the first quadrupole (Ql); however, the urine matrix was subjected to liquid-liquid acidic extraction prior to analysis. The full scan MS/MS product ion spectra demonstrated the capability to confinn the positive urine and can be extended to produce at least three diagnostic ions within 20% relative abundance to fulfil the criteria set by the IOC. The X-calibur program incorporated into the analysis method produces results automati-cally following completion of the analysis. The printed results in concise macro windows assisted in the interpretation of data, consistent with standard IOC screening procedures. | en_US |
| dc.identifier.uri | http://hdl.handle.net/123456789/921 | |
| dc.language.iso | en | en_US |
| dc.subject | Atmospheric pressure | en_US |
| dc.subject | Spectrometry | en_US |
| dc.title | Rapid detection of diuretics by atmospheric pressure chemical ionization (apci) tandem mass spectrometry | en_US |
| dc.type | Thesis | en_US |
Files
License bundle
1 - 1 of 1
Loading...
- Name:
- license.txt
- Size:
- 1.71 KB
- Format:
- Item-specific license agreed upon to submission
- Description: