Comparison of two extraction procedures for determination of drugs of abuse in human saliva by high‐performance liquid chromatography

Abstract

High performance liquid chromatography in combination with diode array detection (HPLC-DAD) was used to determine morphine, 6-acetylmorphine, cocaine, benzoylecgonine, cocaethylene, methadone and 2-ethylene-1,5-dimethyl-3,3,-diphenylpyrrolidine in human saliva. For comparison, samples were prepared by either liquid-liquid extraction in Toxitubes A or microwave-assisted extraction (MAE), by mixing 1 ml of saliva with 10 ml of chloroform and operating at 100 degrees C for 10 min. Acetonitrile and 0.02 m phosphate buffer at pH 6.5 were used as mobile phase in HPLC in gradient mode. The detector response was linear over the drug concentration range of 0.05-2.0 microg ml(-1) in human saliva. The analytical method was validated by determining its precision and accuracy (n = 5), which were lower than 5% as relative standard deviation and 6% as relative error. Limits of detection ranged from 10 to 35 ng ml(-1); mean recoveries of drugs were from 53 to 95% with Toxitubes A and from 83 to 100% with MAE at two different concentrations (0.1 and 1.0 microg ml(-1)). The proposed method was applied to 24 saliva samples from individuals poisoned with opiates and/or cocaine.

Porous silicon mass spectrometry as an alternative confirmatory assay for compliance testing of methadone

“…A commonly noted problem for saliva detection is low saliva production after consumption of certain drugs such as amphetamines. Our technique reduces the likelihood of this being a problem, with just 200 μL required for testing, whereas other techniques can require up to 1 mL …”

Determination of morphine, codeine and 6-monoacetylmorphine in saliva of substance-abuse patients using HPLC/MS methods

“…alternativnih uzoraka sa sve većim značajem za primenu u kliničko-toksikološkoj analizi 4 . Priprema uzoraka salive u svrhu određivnja lekova i sredstava zloupotrebe podrazumeva upotrebu tečno-čvrste 9 , 10-13 , ili tečno-tečne ekstrakcije 14 . Zapremina prikupljenog uzorka salive je često mala, pa se za detekciju supstanci primenjuju tehnike gasne 10 i tečne 9, 11, 12, 15-17 hromatografije sa masenom detekcijom 4 , i tako se obezbeđuje visoka specifič-nost i osetljivost.…”

Sensing cocaine in saliva with attenuated total reflection infrared (ATR-IR) spectroscopy combined with a one-step extraction method

“…It meets the demands of High Pressure Liquid Chromatography with diode array detection (HPLC-DAD). 18 The MAE was found to posses higher recovery rates than Toxi tubes A (Sarsted). Nevertheless this extraction technique involves high temperatures (around 100 • C), centrifuging, drying and reliquifying with the mobile phase of the HPLC device and therefore it needs specially trained staff for the preparation of the samples as well as expensive equipment.…”

“…Nevertheless this extraction technique involves high temperatures (around 100 • C), centrifuging, drying and reliquifying with the mobile phase of the HPLC device and therefore it needs specially trained staff for the preparation of the samples as well as expensive equipment. 18 A simple one-step extraction method which can be applied even in the field would thus be advantegous. Here we present a protocol for sample preparation and measurement which can be miniaturized and taken to field analysis.…”