Automatic on‐line solid‐phase extraction with ultra‐high performance liquid chromatography and tandem mass spectrometry for the determination of ten antipsychotics in human plasma

Abstract

An automatic on-line solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry method was developed for the simultaneous determination of ten antipsychotics in human plasma. The plasma sample after filtration was injected directly into the system without any pretreatment. A Shim-pack MAYI-C8 (G) column was used as a solid-phase extraction column, and all the analytes were separated on a Shim-pack XR-ODS III column with a mobile phase consisting of 0.1% v/v formic acid in water with 5 mM ammonium acetate and acetonitrile. The method features were systematically investigated, including extraction conditions, desorption conditions, the equilibration solution, the valve switching time, and the dilution for column-head stacking. Under the optimized conditions, the whole analysis procedure took only 10 min. The limits of quantitation were in the range of 0.00321-2.75 μg/L and the recoveries ranged from 75.9 to 122%. Compared with the off-line ultra-high performance liquid chromatography and the reported methods, this validated on-line method showed significant advantages such as minimal pretreatment, shortest analysis time, and highest sensitivity. The results indicated that this automatic on-line method was rapid, sensitive, and reliable for the determination of antipsychotics in plasma and could be extended to other target analytes in biological samples.

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

“…Schematic diagram of the novel FSS for the online SPE‐UHPLC (B), from , with the permission of Elsevier. Schematic diagram of the online SPE‐UHPLC using a dual‐dilution strategy (C), from , with the permission of Wiley…”

“…FSS is a strategy based on online dividing a sample solution into fractions by plugs of weak mobile phase, followed by head‐column stacking process. The other configuration of automatic SPE‐UHPLC‐MS/MS system using a dual‐dilution strategy is shown in Figure C . The first dilution that takes place before SPE enables the direct injection of complex samples with minimal pretreatment, and the second dilution that takes place after SPE process and before the UHPLC procedure achieves the direct introduction of large volume of strong eluent into the UHPLC column without causing peak broadening or distortion.…”

“…Apart from the simple water samples, the practical online SPE‐UHPLC technique was also used for the analysis of biological samples, such as milk , urine , plasma , serum , cattle manure‐based biogas , and cells . Recently, an online SPE‐UHPLC method was reported to analyze dried blood spot and the selective, accurate, and precise responses of the target compounds generally meeting the accepted regulated bioanalysis guidelines were observed over the range of 5–1000 ng/mL in whole blood .…”

Comprehensive two-dimensional ion chromatography (2D-IC) coupled to a post-column photochemical fluorescence detection system for determination of neonicotinoids (imidacloprid and clothianidin) in food samples

“…19,38,39,[41][42][43][44] The matrix interferences and analyte loss problems can be resolved by making sample preparation method online with the 2D-IC system just like SPE methods aer making online proved more efficient, versatile, reproducible, selective, reduce labor, human error, costs, solvent and time. [45][46][47][48] Since last two decades, an online column-switching technique for heart-cutting is extensively utilized for complex samples clean-up and concentration to reduce matrix interferences. [49][50][51][52] However, most of the reported online extraction techniques use the mini hydrophobic column as pre-treatment column which unable to complete elimination of matrix interferences from analytes of interest and matrices co-elute and transfer along the analytes of interest in second dimension column.…”

Desenvolvimento de fase monolítica com grupos amino e nano partículas para a determinação de carbidopa, levodopa, benserazida, dopamina e 3-O-metildopa em amostras de plasma de pacientes com a doença de Parkinson por HILIC-MS/MS no modo column switching

“…Sistema column switching em modo foreflush e backflush. Adaptado de(MARCHIONI et al, 2017).Diferentes fases seletivas têm sido utilizadas como coluna 1D no sistema column switching, dentre elas podemos destacar as fases monolíticas (DOMINGUES; SOUZA; QUEIROZ, 2015; MIZUNO; KATAOKA, 2015; LUO; LI; HU, 2017), polímeros molecularmente impressos -MIP -(XU et al, 2010a), materiais de acesso restrito -RAM -(ECKERT;GÖEN, 2014;FAGUNDES et al, 2014;ZHOU et al, 2014;ZHANG et al, 2015; CAGLAR ANDAC, 2016), colunas de fluxo turbulento (CRUTCHFIELD; MARZINKE; CLARKE, HERVIOU et al, 2016;SHIN et al, 2016), imunosorventes (CHAVES; QUEIROZ, 2013), nanotubos de carbono(DE FARIA et al, 2017) e suportes de sílica -C18 -(PARK et al, 2014;PURSLEY et al, 2014;SABAREDZOVIC et al, 2015;XIONG et al, 2015;HÄDENER et al, 2016;ZHONG et al, 2016) A Tabela 2 ilustra algumas aplicações de diferentes fases seletivas na primeira dimensão do sistema LC no modo column switching. Diferentes fases seletivas na primeira dimensão do sistema LC no modo column switching para análise de diferentes analitos em amostras biológicas…”