scholarly journals Microfluidic chips with reversed-phase monoliths for solid phase extraction and on-chip labeling

2012 ◽  
Vol 1261 ◽  
pp. 129-135 ◽  
Author(s):  
Pamela N. Nge ◽  
Jayson V. Pagaduan ◽  
Ming Yu ◽  
Adam T. Woolley
Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2123
Author(s):  
Luboš Fical ◽  
Maria Khalikova ◽  
Hana Kočová Vlčková ◽  
Ivona Lhotská ◽  
Zuzana Hadysová ◽  
...  

Two new ultra-high performance liquid chromatography (UHPLC) methods for analyzing 21 selected antivirals and their metabolites were optimized, including sample preparation step, LC separation conditions, and tandem mass spectrometry detection. Micro-solid phase extraction in pipette tips was used to extract antivirals from the biological material of Hanks balanced salt medium of pH 7.4 and 6.5. These media were used in experiments to evaluate the membrane transport of antiviral drugs. Challenging diversity of physicochemical properties was overcome using combined sorbent composed of C18 and ion exchange moiety, which finally allowed to cover the whole range of tested antivirals. For separation, reversed-phase (RP) chromatography and hydrophilic interaction liquid chromatography (HILIC), were optimized using extensive screening of stationary and mobile phase combinations. Optimized RP-UHPLC separation was carried out using BEH Shield RP18 stationary phase and gradient elution with 25 mmol/L formic acid in acetonitrile and in water. HILIC separation was accomplished with a Cortecs HILIC column and gradient elution with 25 mmol/L ammonium formate pH 3 and acetonitrile. Tandem mass spectrometry (MS/MS) conditions were optimized in both chromatographic modes, but obtained results revealed only a little difference in parameters of capillary voltage and cone voltage. While RP-UHPLC-MS/MS exhibited superior separation selectivity, HILIC-UHPLC-MS/MS has shown substantially higher sensitivity of two orders of magnitude for many compounds. Method validation results indicated that HILIC mode was more suitable for multianalyte methods. Despite better separation selectivity achieved in RP-UHPLC-MS/MS, the matrix effects were noticed while using both chromatographic modes leading to signal enhancement in RP and signal suppression in HILIC.


2008 ◽  
Vol 91 (6) ◽  
pp. 1459-1466 ◽  
Author(s):  
Ji-Ye Hu ◽  
Yu-Chao Zhang ◽  
Hai Yan

Abstract A method for high-performance liquid chromatographic (HPLC) determination of flumorph residues in cucumber, tomato, soil, and natural water was developed and validated. Primary secondary amine or octadecylsilyl (C18) solid-phase extraction cartridges were used for sample preparation. Reversed-phase HPLC with UV detection was used for separation and quantification of the pesticide. The combined cleanup and chromatographic method steps were sensitive and reliable for simultaneous determination of residues of the 2 isomers of flumorph in the studied samples. This method is characterized by recovery >97.9, coefficient of variation <6.2, and limit of quantification of 0.01 mg/kg, in agreement with directives for method validation in residue analysis. Flumorph residues in the samples were further confirmed by HPLC/mass spectrometry. The proposed method is fast, easy to perform, and could be used for monitoring of pesticide residues.


2004 ◽  
Vol 87 (4) ◽  
pp. 937-942 ◽  
Author(s):  
Harumi Oshima ◽  
Eiji Ueno ◽  
Isao Saito ◽  
Hiroshi Matsumoto

Abstract A simple solid-phase extraction (SPE) method was developed for the liquid chromatography (LC) determination of pheophorbide (Phor) a and pyropheophorbide (Pyro) a in health foods such as chlorella, spirulina, etc. The food sample was extracted with 85% (v/v) acetone. The extract was acidified with hydrochloric acid and loaded on a C18 cartridge. After washing with water, Phor a and Pyro a were eluted with the LC mobile phase. Phor a and Pyro a were separated by isocratic reversed-phase LC and quantitated by fluorescence detection. The recoveries for spiked samples of chlorella and the extract were 87.1–102.0%. Commercial health foods (chlorella, spirulina, aloe, kale, Jews mallow, and green tea leaves) were analyzed using the SPE method. The values found for Phor a and Pyro a ranged from 2 to 788 μg/g and from <1 to 24 μg/g, respectively. There was no significant difference between the SPE method and the official method in Japan (spectrophotometry after liquid–liquid extraction). The advantages of the SPE method are the short extraction times, lack of emulsions, and reduced consumption of organic solvents compared with the official method in Japan. The SPE method is considered to be useful for the screening of Phor a and Pyro a in health foods.


2003 ◽  
Vol 86 (6) ◽  
pp. 1160-1163 ◽  
Author(s):  
Thomas A Eisele ◽  
Midori Z Gibson

Abstract A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 μg/kg in an industrial quality assurance laboratory environment.


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