Instrumentation for hand-portable liquid chromatography

被引:50
作者
Sharma, Sonika [1 ]
Plistil, Alex [2 ]
Simpson, Robert S. [2 ]
Liu, Kun [1 ]
Farnsworth, Paul B. [1 ]
Stearns, Stanley D. [2 ]
Lee, Milton L. [1 ]
机构
[1] Brigham Young Univ, Dept Chem & Biochem, Provo, UT 84602 USA
[2] VICI Valco Instruments, Houston, TX 77725 USA
关键词
Liquid chromatography; Hand-portable; Nano-flow pump; Capillary column; On-column detection; UV-absorption; CAPILLARY-ZONE-ELECTROPHORESIS; UV ABSORBENCY DETECTION; ABSORPTION DETECTION; ARRAY DETECTOR; FLOW CELL; PERFORMANCE; MICRO; INJECTION; SYSTEM; ISOTACHOPHORESIS;
D O I
10.1016/j.chroma.2013.12.059
中图分类号
Q5 [生物化学];
学科分类号
071010 ; 081704 ;
摘要
Liquid chromatography (LC) has lagged behind gas chromatography (GC) in developments related to hand-portable instrumentation. In this work, a new battery-operated (24V DC) nano-flow pumping system with a stop-flow injector was developed and integrated with an on-column UV-absorption detector (254 nm) that was reduced in size to an acceptable weight and power usage for field operation. The pumping system, which includes nano-flow pump, stepper motor and high-pressure valve weighs only 1.372 kg (3 Ibs) and can generate up to 110.32 MPa (16,000 psi) pressure. A major advantage of this pump is that it does not employ a splitter, since it was specifically designed for capillary column use. The volume capacity of the pump is 24 mu L, and a sample volume as low as 10 nL can be injected. Flow rate calibration (300 mu L to 6.12 IA per min) was performed, and an accuracy >99.94% was obtained. The percent injection carry-over was found to be low (RSD 0.31%), which makes it practical for quantitative analysis. The detector linear range and limit of detection (LOD) were determined using sodium anthraquinone-2-sulfonate. A linear regression coefficient (R) of 0.9996 was obtained for a plot of log peak area versus log concentration over the range of 3.2 mu M to 6.5 mM, and the LOD (S/N =3) was found to be 7.8 fmol (0.13 mu M). The short term noise of the detector is comparable to commercially available detectors (similar to 10(-5) AU). In this work, the system was tested in the laboratory using regular line power (120V AC) with an AC to DC adapter. Reversed-phase isocratic separations were performed using a 15.5 cm x 75 mu m i.d. fused silica capillary column containing a monolithic stationary phase synthesized from 1,6-hexanediol dimethacrylate. Good retention time repeatability (RSD 0.09-0.74%) was obtained for a mixture containing an unretained marker (i.e., uracil) and a homologous series of alkyl benzenes. (C) 2013 Elsevier B.V. All rights reserved.
引用
收藏
页码:80 / 89
页数:10
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