Rapid monitoring of benzodiazepines in clinical samples by using on-line column switching HPLC

1991 ◽  
Vol 37 (6) ◽  
pp. 804-808 ◽  
Author(s):  
C M Moore ◽  
K Sato ◽  
Y Katsumata

Abstract We have determined routinely administered benzodiazepines and some of their metabolites in clinical samples by using on-line column switching for sample clean-up and reversed-phase high-pressure liquid chromatography (HPLC). The plasma sample is directly injected onto a cyanopropyl (CN) pre-column, washed with buffer, and eluted onto an analytical column (C18, octadecylsilane). Analytical recovery from drug-supplemented plasma samples was greater than 85% for all the benzodiazepines tested. The response of the analytical column varied linearly with drug concentrations over the range 0.01-1 mg/L in plasma, with CVs ranging from 0.3% to 1.8% within-day and 5.5% to 15.7% between days. The detection limit (signal-to-noise ratio greater than 3) was 0.01 mg/L (1 ng on column) for all of the benzodiazepines and their metabolites. The advantages of the technique include the extreme cleanliness of the traces, no requirement for off-line sample preparation, and ease of automation.


2006 ◽  
Vol 42 (5) ◽  
pp. 587-592 ◽  
Author(s):  
Eiichi Yamamoto ◽  
Hatsue Igarashi ◽  
Yoshiaki Sato ◽  
Ikuo Kushida ◽  
Takashi Kato ◽  
...  




1988 ◽  
Vol 34 (1) ◽  
pp. 87-90 ◽  
Author(s):  
K Abe ◽  
R Konaka

Abstract We describe a "high-performance" liquid-chromatographic method for determining 3-methoxy-4-hydroxyphenylethylene glycol (MHPG) in human urine. MHPG is separated on a reversed-phase column with isocratic elution, oxidized with sodium metaperiodate, and its absorbance measured at 365 nm. This method shows higher specificity, less interference for MHPG than methods involving electrochemical or fluorescence detection. Post-column derivatization of MHPG with periodate yields vanillin. The detection limit (twice the signal-to-noise ratio) in urine samples was 0.08 mg/L. Mean analytical recovery was 72%. Within-assay and day-to-day CVs were 2.9% and 6.5%, respectively. Reference intervals for MHPG in 24-h urine from apparently healthy subjects were 0.85-3.24 mg/day for men and 0.63-2.20 mg/day for women. In terms of creatinine excretion, the respective reference intervals were 0.55-1.99 and 0.70-1.96 mg per gram of creatinine.



Author(s):  
Samy Emara ◽  
Maha Kamal ◽  
Ghada Hadad ◽  
Hala ZaaZaa ◽  
Mohamed Abdel Kawi




1993 ◽  
Vol 39 (2) ◽  
pp. 263-271 ◽  
Author(s):  
T Fiskerstrand ◽  
H Refsum ◽  
G Kvalheim ◽  
P M Ueland

Abstract We have developed a modified version of our fully automated column-switching HPLC method for determining total plasma homocysteine based on single-column (reversed-phase) separation. Homocysteine, cysteine, and cysteinylglycine in plasma (total concentrations), acid-precipitated plasma (non-protein-bound concentrations), and urine can be determined. The derivatization and chromatography were performed automatically by a sample processor. The successful separation of all thiol species (within 15 min) was accomplished by accurate adjustment of the pH of the mobile phase to 3.65 (plasma) or 3.50 (acid-precipitated plasma, urine). Maximal fluorescence yield of cysteine, cysteinylglycine, and, to a lesser degree, homocysteine was dependent on optimal concentrations of EDTA and dithioerythritol during reduction (with NaBH4) and derivatization (with monobromobimane). The method is sensitive (detection limit approximately 0.05 pmol) and has a high degree of precision (CV < 5%). The sample output is approximately 70 samples in 24 h. Serum and heparin plasma can also be analyzed. Hemolysis up to approximately 2.0 g/L of hemoglobin did not interfere with the analytical recovery of homocysteine or cysteine. Collection of blood, separation of plasma from whole blood, and acid precipitation must be standardized to obtain reproducible thiol results. Our modifications and the standardization of blood-sampling procedures have substantially improved the method and broadened its applications.





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