Study Of Plasma Analytical Method On The Microchip With Methacrylate Monolithic Column

For the characteristics of analysis integration, automation and miniaturization, remarkable predominance is shown by micro-fluidic chip system in decreasing reagent consumption and shortening analysis time. Sample pretreatment is one of the bottlenecks in the integration process of micro-fluidic chip system, so extensive investigation has been done in this field. For many characteristics of solid phase extraction (SPE) technology, it is very suitable for the pretreatment of complex samples in the integration process of micro-fluidic chip system. Monolithic column is a new kind of material for chromatographic separation and enrichment in recent years, which has the advantages of simple preparation, low backpressure, high resolution and large capacity for solutes. It has been widely applied in SPE and electro-chromatography. So it's very significative to study sample pretreatment technique on micro-fluidic chip using monolithic columns as SPE colums.In this paper, the types, characterization techniques and application actualities of monolithic columns were reviewed. Butyl methacrylate (BMA) and Lauryl methacrylate (LMA) monolithic columns were prepared in pretreated glass tube by in-situ copolymerization of BMA or LMA. EDMA and AIBN were used as cross-linker and initiator, respectively in the reaction process. Moreover, methanol and hexane were used as porogenic reagents. The preparation conditions of LMA monolithic column were optimized by orthogonal experiment. The structure and images of BMA and LMA monolithic columns were characterized by microscopy, scanning electron micrograph (SEM) and infrared spectrum (IR). Results showed that porous and netty BMA and LMA monolithic columns were successfully prepared.BMA monolithic micro-column prepared by in-situ polymerization was combined with micro-fluidic chip to obtain hybrid micro-fluidic chip with BMA monolithic micro-column. For the CL system of K3Fe(CN)6-NaOH-Isoniazied, sampling modes, flow velocity and detection point were discussed. The pretreatment, sampling, impurity elimination and sample elution of hybrid micro-fluidic chip with BMA monolithic micro-column were analyzed. K3Fe(CN)6-NaOH-Isoniazied CL conditions were optimized. Detected column capacity of BMA monolithic micro-column (1mm i.d×2.0cm) was 0.25μg·mg-1. Absorption of BMA monolithic micro-column on the hybrid micro-fluidic chip was detected by chemiluminescence of Isoniazied. The average enrichment efficient was 15.9 and the average absorption efficiency was 79.5% (corresponding RSD was 8.44 %, n=5). Serum sample with Isoniazied was analyzed on the hybrid micro-fluidic chip with BMA monolithic micro-column. Results showed that the average detected value of Isoniazied was 0.344μg and the average recovery was 92.9% (corresponding addition amount was 0.360μg, RSD was 4.72 %, n=3).In addition, urine sample with Cefoperazone Sodium was analyzed on the hybrid micro-fluidic chip with [2-(methacryloyloxy) ethyl] trimethylammonium chloride (META) monolithic micro-column. The average detected value of Cefoperazone Sodium was 0.623μg and the average recovery was 94.3% (corresponding addition amount was 0.660μg, RSD was 2.48 %, n=5).For serum sample with Isoniazied analyzed on the hybrid micro-fluidic chip with BMA monolithic micro-column prepared by in-situ copolymerization and urine sample with Cefoperazone Sodium was analyzed on the hybrid micro-fluidic chip with META monolithic micro-column, the analysis method of drug in blood and rine samples had be established.