Benzylpiperazine BZP - AppNote
October 24, 2014
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Date: 24-OCTOBER-2014 Last Updated: 18-SEPTEMBER-2026
Analysis in Hair Samples using LCMS
An analytical protocol was developed for analysis of Benzylpiperazine in human hair samples. The elucidation of the chromatographic method was challenging due to the polar nature of BZP. The limits of detection / quantification for this method were determined to be 0.05 ng / mg for Benzylpiperazine in hair samples.The method was found to be linear from 0.1 – 10 ng/mg (r2 > 0.999). Recovery of Benzylpiperazine was found to be greater than 95%. Matrix effects were determined to be < 6%.
The concentration of Benzylpiperazine in spiked samples of hair was determined in range from 1.2 – 1.5 ng/mg. The procedure after validation will be useful for laboratories performing routine analysis of drugs of abuse.
Peaks:
A: Benzylpiperazine
177.1386 m/z [M+H]+
B: 5 injections of the sample
Column: Cogent Diamond Hydride™, 4 μm, 100 Å
Catalog No.: 70000-15P-2
Dimensions: 2.1 x 150 mm
Mobile Phase:
— A: DI Water / 0.1% Formic Acid (v/v)
— B: Acetonitrile / 0.1% Formic Acid (v/v)
Gradient:
| Time (minutes) | %B |
|---|---|
| 0 | 80 |
| 3 | 30 |
| 6 | 30 |
| 10 | 80 |
Detection: ESI – POS - Agilent 6210 MSD TOF Mass Spectrometer
Injection vol.: 1 μL
Sample Preparation: Extraction (SPE) was performed on cartridge I (Clean Screen Xcel™ purchased from UCT Bristol, PA, USA), preconditioned with 3 mL of Methanol, 3 mL of DI Water, and 1 mL of pH 6 buffer prior to sample loading. 10 mg samples of hair (controls, and spiked test samples) were digested in 1 mL of 1 M Sodium Hydroxide for 1 hour at 70˚C. The samples were cooled, and 100 µL of Acetic Acid (Glacial) was added.
Each solution was adjusted to pH 6 with 0.1 mM Ammonia and applied to the SPE column. After loading the samples, each sorbent was washed with DI Water, Acetic Acid (0.1 M), and Methanol (3 mL of each, respectively). Each SPE Column was dried and eluted with 3 mL of Methylene Chloride / Isopropanol / Ammonium Hydroxide (78:20:2). After elution, solvents were evaporated and 200 µL of Mobile Phase was added. The samples were used for analysis by LC-MS.
