Liquid chromatography/tandem mass spectrometry for the qualitative and quantitative analysis of illicit drugs and medicines in preserved oral fluid

Abstract

A qualitative and quantitative analytical method was developed for the simultaneous determination of 24 illicit drugs and medicines, in preserved oral fluid samples collected with the StatSure Saliva Sampler collection device. The samples were prepared by liquid-liquid extraction followed by liquid chromatography/tandem mass spectrometry (LC/MS/MS) analysis. The chromatographic separation was performed with an Atlantis T3 (100 x 2.1 mm i.d., 3 microm) reversed-phase column using an acetonitrile/2 mM ammonium formate buffer pH 3.4 gradient and the MS/MS detection was achieved with two precursor-product ion transitions per substance. The method was fully validated, including specificity and capacity of identification, limit of detection (0.2-2.1 microg/L), limit of quantitation (0.8-6.4 microg/L), recovery (34-98%), carryover, linearity (the method was linear in the range 1-200 microg/L), intra-assay precision (coefficient of variance (CV) <20% for 20 microg/L and CV <10% for 100 microg/L) and inter-assay accuracy (mean relative error <15%) and precision (CV <20%). The method showed to be specific and sensitive. It has already been successfully used in four proficiency tests and subsequently applied to oral fluid samples collected from road traffic volunteers in the driving population of Portugal (districts of Lisbon, Coimbra and Porto), within the DRUID project.

Drugs of abuse in oral fluid collected by two different sample kits – Stability testing and validation using ultra performance tandem mass spectrometry analysis

“…The volume of the collected samples is often less than 1 mL, therefore multicomponent methods with low detection limits are needed [2,4]. Developments within analytical technology using liquid chromatography with tandem mass spectrometry (LC-MS/MS) have made it possible to simultaneously quantify several drugs at low concentrations in OF [5][6][7][8][9]. Ultra performance liquid chromatography (UPLC) has been introduced as a replacement for high performance liquid chromatography (HPLC) with potential of faster analysis, less solvent consumption, and improved resolution [10][11][12][13][14], and is considered as a promising technique for analysis of small volumes of OF [15][16][17].…”

Determination of 17 illicit drugs in oral fluid using isotope dilution ultra-high performance liquid chromatography/tandem mass spectrometry with three atmospheric pressure ionizations

“…Simões et al also chose acetonitrile as the organic mobile phase using a Waters Atlantis T3 column, which has the same packing material but in a larger particle size than the HSS T3, to separate 24 illicit drugs and medicines in oral fluid [46]. Similarly, two other studies have also used acetonitrile to analyze illicit drugs in oral fluid with C18 columns [33,47].…”

Assessing Cocaine Abuse Using LC–MS/MS Measurements in Biological Specimens

“…Simões et al [129] have published a method for the analysis of 24 illicit drugs and medicines in preserved oral fluid. The analytes were isolated from the samples via LLE, and the detection limits were 0.5 and 0.9 ng/ml for cocaine and benzoylecgonine respectively.…”