title: 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.
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)).
authors.affiliation: a Shandong Institute for Food and Drug Control , Jinan , China.
authors.forename: Shuyin
authors.initials: S
authors.lastname: Jiang
authors.affiliation: a Shandong Institute for Food and Drug Control , Jinan , China.
authors.forename: Huijie
authors.initials: H
authors.lastname: Tan
authors.affiliation: a Shandong Institute for Food and Drug Control , Jinan , China.
authors.forename: Changchuan
authors.initials: C
authors.lastname: Guo
authors.affiliation: a Shandong Institute for Food and Drug Control , Jinan , China.
authors.forename: Liping
authors.initials: L
authors.lastname: Gong
authors.affiliation: a Shandong Institute for Food and Drug Control , Jinan , China.
authors.forename: Feng
authors.initials: F
authors.lastname: Shi
mesh_terms: D000525:Alprazolam / Q000737:chemistry / Q000302:isolation & purification; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation / Q000379:methods*; D002998:Clonazepam / Q000737:chemistry / Q000302:isolation & purification; D003975:Diazepam / Q000737:chemistry / Q000302:isolation & purification; D019587:Dietary Supplements / Q000032:analysis*; D004340:Drug Contamination; D059022:Food Safety; D006801:Humans; D006993:Hypnotics and Sedatives / Q000737:chemistry / Q000302:isolation & purification*; D057230:Limit of Detection; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry / Q000295:instrumentation / Q000379:methods*
chemical_list: D006993:Hypnotics and Sedatives; D002998:Clonazepam; D003975:Diazepam; D000525:Alprazolam
keywords: Orbitrap; adulteration; detection; dietary supplements; screening; sedative-hypnotics