Molecularly imprinted solid-phase extraction for the selective determination of methamphetamine, amphetamine, and methylenedioxyphenylalkylamine designer drugs in human whole blood by gas chromatography-mass spectrometry

• Published in: Journal of separation science 2012-03, Vol.35 (5-6), p.726-733
• Main Authors: Kumazawa, Takeshi, Hasegawa, Chika, Hara, Kenji, Uchigasaki, Seisaku, Lee, Xiao-Pen, Seno, Hiroshi, Suzuki, Osamu, Sato, Keizo
• Format: Article
• Language: English
• Subjects: 3,4-Methylenedioxyamphetamine - analogs & derivatives; 3,4-Methylenedioxyamphetamine - blood; 3,4-Methylenedioxyamphetamine - isolation & purification; Adsorption; Amphetamine - blood; Amphetamine - isolation & purification; Amphetamines; Amphetamines - blood; Amphetamines - isolation & purification; Amphetamines / GC; Biological and medical sciences; Blood; Designer Drugs - analysis; Designer Drugs - isolation & purification; Drug addictions; Drugs; Extraction; Gas Chromatography-Mass Spectrometry - methods; Human; Human whole blood; Humans; Medical sciences; Methamphetamine; Molecular Imprinting; Molecularly imprinted polymer solid-phase extraction; Polymers - chemical synthesis; Polymers - chemistry; Solid Phase Extraction - instrumentation; Solid Phase Extraction - methods; Spectrometry; Spectroscopy; Toxicology
• ISSN: 1615-9306; 1615-9314
• DOI: 10.1002/jssc.201100924

A novel method is described for the extraction of methamphetamine, amphetamine, and methylenedioxyphenylalkylamine designer drugs, such as 3,4‐methylenedioxy‐methamphetamine, 3,4‐methylenedioxyamphetamine, 3,4‐methylenedioxyethylamphetamine, N‐methyl‐1‐(3,4‐methylenedioxyphenyl)‐2‐butanamine, and 3,4‐(methylenedioxyphenyl)‐2‐butanamine, from human whole blood using molecularly imprinted solid‐phase extraction as highly selective sample clean‐up technique. Whole blood samples were diluted with 10mmol/L ammonium acetate (pH 8.6) and applied to a SupelMIP‐Amphetamine molecularly imprinted solid‐phase extraction cartridge. The cartridge was then washed to eliminate interferences, and the amphetamines of interest were eluted with formic acid/methanol (1:100, v/v). After derivatization with trifluoroacetic anhydride, the analytes were quantified using gas chromatography‐mass spectrometry. Recoveries of the seven amphetamines spiked into whole blood were 89.1‐102%. The limits of quantification for each compound in 200 |mL of whole blood were between 0.25 and 1.0 ng. The maximum intra‐ and inter‐day coefficients of variation were 9.96 and 13.8%, respectively. The results show that methamphetamine, amphetamine, and methylenedioxyphenylalkyl‐amine designer drugs can be efficiently extracted from crude biological samples such as whole blood by molecularly imprinted solid‐phase extraction with good reproducibility. This extraction method will be useful for the pretreatment of human samples before gas chromatography‐mass spectrometry.