色谱法
化学
固相萃取
液相色谱-质谱法中的离子抑制
墨盒
检出限
整体
萃取(化学)
质谱法
吸附剂
基质(化学分析)
串联质谱法
整体式高效液相色谱柱
可待因
液相色谱-质谱法
高效液相色谱法
吸附
吗啡
材料科学
催化作用
药理学
医学
有机化学
冶金
生物化学
作者
Tarang Nema,Eric Chun Yong Chan,Paul C. Ho
摘要
Presence of matrix ions could negatively affect the sensitivity and selectivity of liquid chromatography-tandem mass spectrometer (LC-MS/MS). In this study, the efficiency of a miniaturized silica monolithic cartridge in reducing matrix ions was demonstrated in the simultaneous extraction of morphine and codeine from urine samples for quantification with LC-MS. The miniaturized silica monolith with hydroxyl groups present on the largely exposed surface area function as a weak cation exchanger for solid phase extraction (SPE). The miniaturized silica cartridge in 1 cm diameter and 0.5 cm length was housed in a 2-ml syringe fixed over a SPE vacuum manifold for extraction. The cleaning effectiveness of the cartridge was confirmed by osmometer, atomic absorption spectrometer, LC-MS and GC-TOFMS. The drugs were efficiently extracted from urine samples with recoveries ranging from 86% to 114%. The extracted analytes, after concentration and reconstitution, were quantified using LC-MS/MS. The limits of detection for morphine and codeine were 2 ng/ml and 1 ng/mL, respectively. The relative standard deviations of measurements ranged from 3% to 12%. The monolithic sorbent offered good linearity with correlation coefficients > 0.99, over a concentration range of 50-500 ng/ml. The silica monolithic cartridge was found to be more robust than the particle-based packed sorbent and also the commercial cartridge with regards to its recyclability and repeated usage with minimal loss in efficiency. Our study demonstrated the efficiency of the miniaturized silica monolith for removal of matrix ions and extraction of drugs of abuse in urinary screening.
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