1. Development of an ultra-high-performance liquid chromatography coupled to high-resolution quadrupole-Orbitrap mass spectrometry method for the rapid detection and confirmation of illegal adulterated sedative-hypnotics in dietary supplements.
- Author
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Jiang S, Tan H, Guo C, Gong L, and Shi F
- Subjects
- Alprazolam chemistry, Alprazolam isolation & purification, Chromatography, High Pressure Liquid instrumentation, Clonazepam chemistry, Clonazepam isolation & purification, Diazepam chemistry, Diazepam isolation & purification, Food Safety, Humans, Hypnotics and Sedatives chemistry, Limit of Detection, Reproducibility of Results, Tandem Mass Spectrometry instrumentation, Chromatography, High Pressure Liquid methods, Dietary Supplements analysis, Drug Contamination, Hypnotics and Sedatives isolation & purification, Tandem Mass Spectrometry methods
- Abstract
A novel method using ultra-high performance liquid chromatography coupled to hybrid quadrupole-Orbitrap high-resolution mass spectrometry (UHPLC-Q-Orbitrap) was developed and validated for the simultaneous screening, identification and quantification of sedative-hypnotics in dietary supplements. Chromatographic conditions were optimised and a full data-dependent MS(2) scan (MS/dd-MS(2)) in positive and negative ion mode was used. A single injection was sufficient to perform the simultaneous screening and identification/quantification of samples. The response showed a good linear relationship with analyte concentrations over wide ranges (e.g., 1.0-1000 ng g(-1) for diazepam) with all the determination coefficients (r(2)) > 0.9985. The method was validated, obtaining accuracy (intra- and inter-day) in the range of 94.5-105.3% and precision (intra- and inter-day) in the range of 0.4-8.9%, respectively. The detection limits (LODs) were in the range of 0.3-1.0 ng g(-1) for different analytes. Recoveries were performed and ranged from 74.1% to 90.2%, while all matrix effects were over the range of 85.4-93.6%. Finally, this method was used to detect sedative-hypnotics in commercial dietary supplements. Of a total of 45 batches of dietary supplements, only three batches were found to be positive samples with concentrations of diazepam, clonazepam and alprazolam at high levels (≥ 8.22 mg g(-1)).
- Published
- 2015
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