Automatic analytical approach for the determination of 12 illicit drugs and nicotine metabolites in wastewater using on-line SPE-UHPLC-MS/MS
- Author:
Jingyuan WANG
1
,
2
;
Likai QI
;
Chenzhi HOU
;
Tingting ZHANG
;
Mengyi CHEN
;
Haitao MENG
;
Mengxiang SU
;
Hui XU
;
Zhendong HUA
;
Youmei WANG
;
Bin DI
Author Information
1. Department of Pharmacy,China Pharmaceutical University,Nanjing,210009,China
2. China National Narcotics Control Commission-China Pharmaceutical University Joint Laboratory on Key Technologies of Narcotics Control,Nanjing,210009,China
- Keywords:
Illicit drugs and metabolites;
Wastewater analysis;
On-line solid phase extraction;
Ultra-high-performance liquid;
chromatography;
Mass spectrometry
- From:
Journal of Pharmaceutical Analysis
2021;11(6):739-745
- CountryChina
- Language:Chinese
-
Abstract:
In this study,we developed a novel on-line solid phase extraction (SPE)-ultra-high-performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS)-based analytical method for simulta-neously quantifying 12 illicit drugs and metabolites (methamphetamine,amphetamine,morphine,co-deine,6-monoacetylmorphine,benzoylecgonine,3,4-methylenedioxymethamphetamine,3,4-methylenedioxyamphetamine,cocaine,ketamine,norketamine,and methcathinone) and cotinine(COT) in wastewater samples.The analysis was performed by loading 2 mL of the sample onto an Oasis hydrophilic-lipophilic balance cartridge and using a cleanup step (5％ methanol) to eliminate interference with a total run time of 13 min.The isotope-labeled internal standard method was used to quantify the target substances and correct for unavoidable losses and matrix effects during the on-line SPE process.Typical analytical characteristics used for method validation were sensitivity,linearity,precision,repeatability,recovery,and matrix effects.The limit of detection (LOD) and limit of quantification (LOQ)of each target were set at 0.20 ng/L and 0.50 ng/L,respectively.The linearity was between 0.5 ng/L and 250 ng/L,except for that of COT.The intra-and inter-day precisions were ＜10.45％ and 25.64％,respec-tively,and the relative recovery ranged from 83.74％ to 162.26％.The method was used to analyze various wastewater samples from 33 cities in China,and the results were compared with the experimental re-suits of identical samples analyzed using off-line SPE.The difference rate was between 19.91％and-20.44％,and the error range could be considered acceptable.These findings showed that on-line SPE is a suitable alternative to off-line SPE for the analysis of illicit drugs in samples.
