Gas chromatographic determination of midazolam in low-volume plasma samples
| Autor: | Stefan Masur, Berndt-Ingo Podkowik |
|---|---|
| Rok vydání: | 1996 |
| Předmět: |
Detection limit
Analyte Chromatography Chromatography Gas Chemistry Microchemistry Midazolam Extraction (chemistry) Analytical chemistry General Chemistry Hydrogen-Ion Concentration Mass spectrometry Sensitivity and Specificity Rats Liquid–liquid extraction Blood plasma Animals Humans Hypnotics and Sedatives Gas chromatography Quantitative analysis (chemistry) Adjuvants Anesthesia |
| Zdroj: | Journal of chromatography. B, Biomedical applications. 681(2) |
| ISSN: | 1572-6495 |
| Popis: | A gas chromatographic method for the sensitive determination of midazolam in plasma volumes as low as 40 microliters was developed, utilizing clinazolam as the internal standard. After liquid-liquid extraction at basic pH into 1-chlorobutane-dichloromethane (96:4) a 2- to 4-microliters portion of the reconstituted extract was injected under electronic pressure control onto a 12 m x 0.2 mm I.D. methyl silicone capillary column, and was exposed to a three-step temperature program from 120 to 310 degrees C, to separate the analytes from the plasma constituents. The compound of interest was identified and quantified by means of a mass-selective detector. The assay was linear from 10 to 500 ng/ml using 40 microliters of plasma (limit of quantification: 10 ng/ml) and was linear from 0.25 to 100 ng/ml using 500 microliters of plasma (limit of quantification: 0.25 ng/ml). The intra-day precision for the 40-microliters aliquots varied from 2.2 to 6.6%, the corresponding accuracy from -7.4 to -4.4%; the inter-day precision ranged from 5 to 7.2% and the corresponding accuracy from -7.2 to -5.1%. |
| Databáze: | OpenAIRE |
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