应用分子印记固相萃取法结合高效液相色谱测定池塘水及三种鱼肉中

本文合成并评价了一种作为固相萃取材料的分子印记聚合物,并结合高效液相色谱,有效测定了池塘水及三种鱼肉中磺胺甲基嘧啶的含量。在该聚合物中,模板分子为磺胺甲基嘧啶,功能单体为甲基丙烯酸,交联剂为二甲基丙烯酸乙二醇酯,溶剂为四氢呋喃。通过红外及静态吸附等方法,对

Analysis of Sulfamerazine in Pond Water and Several Fishes by High-Performance Liquid Chromatography Using a

Molecularly Imprinted Solid-Phase Extraction

Guo Linyuan，Jiang Xiaoman，Yang Cailing，Zhang Haixia *

Department of Chemistry，Lanzhou University，Lanzhou（730000）

E-mail：

Abstract

The synthesis and evaluation of a molecularly imprinted polymer (MIP) as a selective solid-phase extraction sorbent, coupled to high-performance liquid chromatography (HPLC), for the efficient determination of sulfamerazine (SMR) in pond water and three fishes are reported. The polymer was prepared using SMR as the template molecule, methacrylic acid as the functional monomer and ethylene glycol dimethacrylate as the cross-linking monomer in the presence of tetrahydrofuran as the solvent. The SMR-imprinted polymers and non-imprinted polymers were characterized by FT-IR and the static adsorption experiments. The prepared SMR-imprinted material showed high adsorption capacity, significant selectivity and good site accessibility. The maximum static adsorption capacity of the SMR-imprinted and non-imprinted material for SMR was 108.8 and 79.6 mg g-1, respectively. The relatively selective factor value of this SMR-imprinted material was 1.6. Several parameters influencing the solid-phase extraction process were optimized. At last, the SMR-imprinted polymers were used as the sorbent in solid-phase extraction to determine SMR in pond water and three fishes with satisfactory recovery. The limit of detection (LOD) for SMR was 1 ng g-1 and the limit of quantitation (LOQ) was 3.5 ng g-1. Keywords：Molecularly imprinted polymers (MIPs) ；Solid-phase extraction；Sulfamerazine (SMR) ；High-Performance Liquid Chromatography (HPLC)

1． Introduction

Molecularly imprinted polymers (MIPs) are an artificially synthesized macromolecular material, which is effective in encoding molecular information (shape, size and functional groups orientation) in bulk materials [1, 2]. In the last few years, MIPs were widely used for the selective enrichment and pretreatment of target compounds existing in complex matrix. And molecular imprinting technology has been expanded to the field of environmental analysis [3-7]. The synthesis of molecularly imprinted polymers (MIPs) involves the formation of a complex between a template molecule and the functional monomers in an appropriate solvent. After polymerization, the template molecule is removed and leaving micro cavities that are complementary to the template molecule. The advantages presented by imprinting techniques are numerous, as these polymeric materials are robust to extremes of temperature and pH, and can retain their recognition properties over periods of several years [8]. Their reusability and shorter preparation times are also their obvious advantages. Great efforts have been directed to apply the molecular recognition capability of MIPs to solid phase extraction [9, 10].

Solid-phase extraction (SPE) has become a routine tool in many laboratories for pre- concentration and/or clean-up steps in the analysis of numerous environmental and bioanalytical samples [11-15]. Due to the popularity of SPE, new sorbents have appeared as alternative to conventional sorbents with the aim of achieving a more and more selective preconcentration of target analytes. Thus, molecularly imprinted polymers (MIPs), relied on affinity interactions and potentially offer a higher degree of sample clean-up efficiency than that achieved using conventional type SPE sorbents [16], appear as excellent candidates to accomplish this requirement [17]. The application of MIP technology to solid-phase extraction (MISPE) has been used for both biological and environmental samples and has been reviewed in detail [18-21]. The majority of studies into MISPE have used cartridges or columns off-line from the downstream analytical separation [22]. Nearly all the study published about MIPs as sorbents in solid-phase extraction (MISPE) has been generated in an

本文合成并评价了一种作为固相萃取材料的分子印记聚合物,并结合高效液相色谱,有效测定了池塘水及三种鱼肉中磺胺甲基嘧啶的含量。在该聚合物中,模板分子为磺胺甲基嘧啶,功能单体为甲基丙烯酸,交联剂为二甲基丙烯酸乙二醇酯,溶剂为四氢呋喃。通过红外及静态吸附等方法,对

off-line mode [23-26]. Most of these methods are based on HPLC cooperated with various sample pretreatment techniques.

Sulfonamides, as veterinary drugs, are widely used to treat and prevent infections, such as gastrointestinal and respiratory infections [27-30], and to promote growth of livestock and fish [31-36]. Sulfonamide residues in food are an important concern, due to the possibility of risk to human health, such as resistance development and toxicity [37]. When inappropriate abusive antibiotic-based treatments are applied to treat livestock diseases, undesirable residues can remain in both the animal tissues. These residues are a great public health concern due to the risk of developing drug resistance, which leads to an inefficiency of this medicine for therapeutic use. Because of concerns they posed on human health and for regulatory purposes, the European Commission (EC) adopted a maximum residue level (MRL) of 100µg kg-1 of sulfonamide in foodstuffs of animal origin [38, 39]. Therefore, the determination of such residues in meat and other animal by-products has become an important task [40].

The current analytical methods for determination of SMR in waste water and tissues include capillary electrophoresis [41], liquid chromatography [42-47] and mass spectrometry [48, 49]. However, there is an absence of effective screening and quantitative meth …… 此处隐藏：30452字，全部文档内容请下载后查看。喜欢就下载吧 ……