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1,4-Benzodiazepines in Urine Analyzed by LCMS.

Reference Number: AA-02323 Created: 05/08/2014 12:38 PM Last Updated: 09/17/2020 03:25 PM

LC-MS method with SPE


1,4-Benzodiazepinein Urine

Peak: 1. Temazepam 301.0739 m/z [M+H]+
         2. Diazepam 285.0790 [M+H]+
         3. Nordiazepam 271.0633 [M+H]+

         4. Midazolam 326.0855 [M+H]+

Method Conditions
 Column: Cogen Diol, 4.4µm 1 00Å
 Catalog No.: 40060-05P-2
 Dimensions: 2.1 x 50 mm
 Solvents: A: DI  H20  /  0 .1% formic  Acid (v/v)
                 B: Acetonitrile/ 0.1% formic Acid (v/v)
 Gradient: (Fig. A) (Fig. B)
         

       time (min.)     %B         time (min.)    %B        
                    0       85            0               10
                    6       70            6               10
                    7       20            7               50
                    9       20            9               50
                    10     85            10             10

 Post time: 3 min
 Injection vol.: 1 µL 
 Flow rate: 0.4 ml/min 
 Detection: ESI – POS  Perki Elme AxIO 2 TOF mass spectrometer
 Flow rate: 0.4 ml/min 
       Samples: Extraction method: Spike urine  sampl was loaded into SPcartridge I (Clean Screen Xcel purchased from UCT BristolPA, USA) and eluted with 0.78 mL of acetonitrile, 200 microL of 2-propanol, 20 microL of ammonia. After the elution, thsampl wadried unde N2 gas and dissolved in 100 microof 50% methanol / 50% DI H2O / 0.1% formic acid. 

            Before injection, the 10 ppm spiked sample was filtered through a 0 .45µm nylon syringe filter (MicroSolv Tech Corp).

Discussion: The Cogent Diol column was used in analysis  of 1,4-benzodiazepines in urine  samples  after SPE extraction using  two types of retention modes.  Four  available compounds were  well  retained and separated in both modes;  however, the retention order was changed depending on the gradient used. It is worth noticing that the peak intensities were  three times higher when  using  Gradient A (ANP mode) compared to Gradient B (RP mode).

Notes:
Benzodiazepines are prescribed for conditions such as anxiety disorders, insomnia, seizures,  and alcohol withdrawal. However, they also have potential for abuse as recreational drugs.

Click HERE for Cogent Diol HPLC Column Ordering Information.

     © Copyright MicroSolv Technology Corporation, all rights reserved.

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