Development of a Novel Sensitive and Fast Semi-Covalent Molecularly Imprinted Polymer-Based Magnetic Dispersive Solid-Phase Extraction Method (MIP-MDSPE) for Cholesterol Determination in Milk Samples

IF 1.3 4区 化学 Q3 CHEMISTRY, MULTIDISCIPLINARY
Luciane Effting, Alesandro Bail, M. Segatelli, C. Tarley
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引用次数: 1

Abstract

In the present study, a novel magnetic dispersive solid-phase extraction method using molecularly imprinted polymer synthesized through semi-covalent imprinting approach was developed for cholesterol (CHO) determination in milk samples by high-performance liquid chromatography with diode array detector (HPLC-DAD). The adsorbent named Fe3O4/SiO2/MIP (MIP: molecularly imprinted polymers) was prepared through sol-gel polymerization of 3-(triethoxysilyl)propyl isocyanate (ICPTES) covalently bonded to CHO with tetraethoxysilane (TEOS), in the presence of Fe3O4/SiO2 particles. The adsorbent was characterized by attenuated total reflection Fourier transform infrared (ATR-FTIR), X-ray diffraction (XRD), dynamic light scattering (DLS) and scanning electron microscopy (SEM). The proposed molecularly imprinted polymer-based magnetic dispersive solid-phase extraction method (MIP-MDSPE) was based on vortex-assisted preconcentration of 10.0 mL of CHO solution in chloroform as donor phase using 10.0 mg of Fe3O4/SiO2/MIP during 60 s. After this step, the magnetic particles were collected using a permanent magnet and the vortex-assisted elution was carried with 500 µL of ethanol during 180 s. A wide analytical curve ranging from 38.5 to 25000 µg L-1 (determination coefficient (R2 ) = 0.998) and low limits of detection (LOD) and quantification (LOQ) 11.5 and 38.5 µg L-1, respectively, were obtained. Milk samples (whole and reduced-fat milk) were subjected to MIP-MDSPE method after saponification reaction followed by CHO extraction with chloroform. Using external calibration, the CHO concentration ranged from 99.2 (reduced-fat milk) to 397.6 mg kg-1 (whole milk) and the accuracy was attested by addition and recovery tests (92 to 97%).
基于半共价分子印迹聚合物的磁分散固相萃取法(MIP-MDSPE)测定牛奶样品中胆固醇的研究
采用半共价印迹法合成分子印迹聚合物,建立了一种新型的磁分散固相萃取方法,用于高效液相色谱-二极管阵列检测器(HPLC-DAD)测定牛奶样品中的胆固醇(CHO)。在Fe3O4/SiO2颗粒存在下,将3-(三乙氧基硅基)异氰酸丙酯(ICPTES)与四乙氧基硅烷(TEOS)共价结合CHO,通过溶胶-凝胶聚合制备了Fe3O4/SiO2/MIP (MIP:分子印迹聚合物)吸附剂。采用衰减全反射傅里叶变换红外(ATR-FTIR)、x射线衍射(XRD)、动态光散射(DLS)和扫描电镜(SEM)对吸附剂进行了表征。本文提出的分子印迹聚合物磁分散固相萃取方法(MIP- mdspe)是基于以10.0 mg Fe3O4/SiO2/MIP为供相,以氯仿为供体,以10.0 mL CHO溶液为供体,在60 s内进行涡旋辅助预富集。该步骤完成后,用永磁体收集磁性颗粒,用500µL乙醇在180 s内进行涡流辅助洗脱。在38.5 ~ 25000µg L-1范围内(决定系数(R2) = 0.998),低检出限(LOD) 11.5µg L-1,定量限(LOQ) 38.5µg L-1。牛奶样品(全脂牛奶和脱脂牛奶)经皂化反应后,用氯仿提取CHO,采用MIP-MDSPE法。通过外部校准,CHO浓度范围为99.2(低脂牛奶)~ 397.6 mg kg-1(全脂牛奶),并通过添加和回收率试验证明其准确性(92% ~ 97%)。
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来源期刊
CiteScore
2.90
自引率
7.10%
发文量
99
审稿时长
3.4 months
期刊介绍: The Journal of the Brazilian Chemical Society embraces all aspects of chemistry except education, philosophy and history of chemistry. It is a medium for reporting selected original and significant contributions to new chemical knowledge.
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