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Analytica Chimica Acta (v.690, #2)

Editorial Board (pp. i).

Magnetoanalysis of micro/nanoparticles: A review by Masayori Suwa; Hitoshi Watarai (pp. 137-147).
Application of magnetic field on the separation and analysis of nano/microparticles is a growing subject in analytical separation chemistry. The migration phenomenon of a particle under inhomogeneous magnetic field is called magnetophoresis. The migration velocity depends on the magnetic susceptibility and the size of a particle. Therefore, magnetophoresis allows us to determine the magnetic susceptibility of particles, and to separate particles based on the magnetic properties. Magnetic separation of ferromagnetic particles in liquid has been utilized for a long time. For example, a high gradient magnetic separation under the non-uniform magnetic field generated by ferromagnetic mesh has been utilized in a wide region from chemical industry to bioscience. Recent progress on magnetic nanoparticles and microfluidic devices has made it possible to extend the range of application. Furthermore, it has been demonstrated that the very sensitive measurement of the magnetic susceptibility of microparticles can be performed by observing magnetophoretic velocity. In this review, we mainly introduce novel separation and detection methods based on magnetophoresis, which have been invented in this decade, and then new principles of particle migration under magnetic field are presented.

Keywords: Magnetophoresis; Magnetic separation; Magnetic force; Nano/microparticles


Chromatographic separation techniques and data handling methods for herbal fingerprints: A review by Christophe Tistaert; Bieke Dejaegher; Yvan Vander Heyden (pp. 148-161).
As herbal medicines have an important position in health care systems worldwide, their current assessment and quality control are a major bottleneck. Over the past decade, major steps were taken not only to improve the quality of the herbal products but also to develop analytical methods ensuring their quality. Nowadays, chromatographic fingerprinting is the generally accepted technique for the assessment and quality control of herbal products. This paper briefly considers the evolution of the regulations and guidelines on the quality control of herbal medicines, and reviews the established analytical techniques for herbal fingerprinting with an emphasis on the most recent developments, such as miniaturized techniques, new stationary phases, analysis at high temperatures and multi-dimensional chromatography. Accessory to the new analytical techniques, the chemometric data handling techniques applied are discussed. Chemometrics provide scientists with useful tools in understanding the huge amounts of data generated by the analytical advances and prove to be valuable for quality control, classification and modelling of, and discrimination between herbal fingerprints.

Keywords: Fingerprints; Chromatography; Data analysis; Herbal species


Baseline correction combined partial least squares algorithm and its application in on-line Fourier transform infrared quantitative analysis by Jiangtao Peng; Silong Peng; Qiong Xie; Jiping Wei (pp. 162-168).
In order to eliminate the lower order polynomial interferences, a new quantitative calibration algorithm “Baseline Correction Combined Partial Least Squares (BCC-PLS)”, which combines baseline correction and conventional PLS, is proposed. By embedding baseline correction constraints into PLS weights selection, the proposed calibration algorithm overcomes the uncertainty in baseline correction and can meet the requirement of on-line attenuated total reflectance Fourier transform infrared (ATR-FTIR) quantitative analysis. The effectiveness of the algorithm is evaluated by the analysis of glucose and marzipan ATR-FTIR spectra. BCC-PLS algorithm shows improved prediction performance over PLS. The root mean square error of cross-validation (RMSECV) on marzipan spectra for the prediction of the moisture is found to be 0.53%, w/w (range 7–19%). The sugar content is predicted with a RMSECV of 2.04%, w/w (range 33–68%).

Keywords: Attenuated total reflectance Fourier transform infrared; Baseline correction; Partial Least Squares; Weight selection


Ionic liquid-functionalized graphene as modifier for electrochemical and electrocatalytic improvement: Comparison of different carbon electrodes by Meng Du; Tao Yang; Suyan Ma; Changzhi Zhao; Kui Jiao (pp. 169-174).
Electrochemical activities of typically electrochemical targets at three kinds of modified carbon electrodes, i.e. carbon ionic liquid electrode (CILE), graphene/carbon paste electrode (CPE), and ionic liquid-functionalized graphene (IL-graphene)/CPE, were compared in detail. The redox processes of the probes at IL-graphene/CPE were faster than those at CILE and graphene/CPE from cyclic voltammetry. An electrochemical method for the simultaneous determination of guanine and adenine was described with detection limits of 6.5×10−8molL−1 (guanine) and 3.2×10−8molL−1 (adenine). Single A→G mutation of sequence-specific DNA could be discriminated by the IL-graphene/CPE.

Keywords: Graphene; Ionic liquid; DNA; Electrocatalysis; Voltammetry


Novel amperometric sensor using metolcarb-imprinted film as the recognition element on a gold electrode and its application by Ming-Fei Pan; Guo-Zhen Fang; Bing Liu; Kun Qian; Shuo Wang (pp. 175-181).
A molecularly imprinted film is electrochemically synthesized on a gold electrode using cyclic voltammetry to electropolymerize o-aminothiophenol in the presence of metolcarb (MTMC). The mechanism of the imprinting process and a number of factors affecting the activity of the imprinted film are discussed and optimized. Scanning electron microscope observations and binding measurements have proved that an MTMC-imprinted film (with a thickness of nearly 100nm) was formed on the surface of the gold electrode. The film exhibited high binding affinity and selectivity towards the template MTMC, as well as good penetrability, reproducibility and stability. A novel amperometry sensor using the imprinted film as recognition element was developed for MTMC determination in food samples. Under the experimental conditions, the MTMC standard is linear within the concentration range studied ( r2=0.9906). The limit of detection ( S/ N=3) of the modified electrode was achieved to 1.34×10−8molL−1. Recoveries of MTMC from spiked apple juice, cabbage and cucumber samples for the developed electrochemical assay ranged from 94.80% to 102.43%, which was with great correlation coefficient (0.9929) with results from high-performance liquid chromatography. In practical application, the prepared amperometric sensor also showed good reproducibility and long lifetime for storage. The research in this study has offered a rapid, accurate and sensitive electrochemical method for quantitative determination of MTMC in food products.

Keywords: Metolcarb; Molecularly imprinted film; Electropolymerization; Chronoamperometry; Sensor


Determination of hexavalent chromium (Cr(VI)) in plastics using organic-assisted alkaline extraction by Jeong Sook Kim; Young Rak Choi; Youn Sung Kim; Yeo Jin Lee; Joung Ho Ko; So Young Kwon; Soo Bong Heo (pp. 182-189).
An organic-assisted alkaline extraction method was developed for the determination of hexavalent chromium (Cr(VI)) in plastics. The solubilization of polymer as a pre-step of the alkaline extraction provided good extraction efficiency of Cr(VI) from the sample. The optimization of the experimental conditions affecting the extraction and UV–vis spectrophotometric analysis was accomplished by evaluating the recovery rate of Cr(VI) through the analysis of Cr(VI) in in-house polymer reference materials (RMs). With the proposed method, most of the Cr(VI) in polymers was released within a short extraction time of 30min and the Cr(III)-DPCO complex can be kept stable for 24h. The heating for the extraction of the Cr(VI) was not necessary. The optimal pH of the final solution was fixed at 2.0. The proposed extraction method was applied successfully for the determination of Cr(III) and Cr(VI) in spiked samples. The practical applicability of this new method was evaluated through the analysis of Cr(VI) in in-house polymer RMs. The good linearity was demonstrated at desired concentrations of the range 0–3.3mgL−1. The detection limits were quite low, varying from 0.0061 to 0.0285mgL−1. The recovery of Cr(VI) was between 97 and 106%, and the relative standard deviation (R.S.D.) was below 6%.

Keywords: Hexavalent chromium (Cr(VI)); Alkaline extraction; In-house reference materials


A new biosynthetic tracer for the inline measurement of virus retention in membrane processes: Part I – Synthesis protocol by L. Soussan; C. Guigui; S. Alfenore; S. Mathe; C. Cabassud (pp. 190-198).
In this study, a new biosynthetic tracer was developed to characterize the virus retention dynamics of membrane systems. This new tracer is a modified bacteriophage obtained by the grafting of enzymatic probes to an MS2 bacteriophage, one of the smallest non-pathogenic bacteria viruses, with an average diameter of about 30nm. A protocol for the synthesis and purification of this new tracer was developed in this work. The production of this biosynthetic tracer was first qualitatively shown by a chromatographic characterization and an enzymatic test. The average number of probes grafted per phage was then quantified for three batches of tracers made from the same native phage suspension and the same batch of enzymatic probes. This quantification demonstrated the reproducibility of the synthesis protocol developed.

Keywords: Virus retention; Biosynthetic tracer; MS2 bacteriophage; Probes; Enzymatic assay; Chromatography


A new biosynthetic tracer for the inline measurement of virus retention in membrane processes: Part II. Biochemical and physicochemical characterizations of the new tracer by L. Soussan; C. Guigui; S. Alfenore; S. Mathe; C. Cabassud (pp. 199-208).
In a previous work, a reproducible procedure to produce a new biosynthetic tracer was developed. This new tracer is an MS2 bacteriophage with enzymatic probes grafted on its surface, which can induce enzymatic activity of the tracer. In this paper, the biochemical and physicochemical characteristics of this new tracer are determined. A protocol was developed to determine the specific enzymatic activity kcatTRACER of the tracer, which was found to be 2.93±0.78×104min−1 on average. Physicochemical characterizations of this new tracer showed that it is representative of viruses and may thus be used as a virus surrogate to assess the virus retention of membrane systems inline. Notably, the mean diameter and molecular weight of the tracer were found to be respectively 64.1±0.3nm and 12140±3654kDa, which are within the size and molecular weight ranges of pathogenic viruses carried by water. The tracer surface was also studied and revealed the considerable porosity of the grafted probe layer, with a mean porosity of 88%, which could explain why the zeta potential of the tracers (−14.34±1.66mV) was nearly the same as that of the native MS2 phages. Finally, a comparison between filtration of the reference microorganism used for membrane performance assessment (the MS2 phage) and the tracer suspensions showed the same filtration behaviour.

Keywords: Abbreviations; HPLC–SEC; high performance liquid chromatography–size exclusion chromatography; HRP; horseradish peroxidase; T; i; the peak or the fraction of tracers at the; i; th HPLC–SEC purification step; S; i; the peak or the fraction of free probes at the; i; th HPLC–SEC purification step; 〈; 〉; the mean values of the terms concernedBiosynthetic tracer; Virus surrogate; Enzymatic activity; Physicochemical properties; Membrane filtration


Quantitation of the glutathione in human peripheral blood by matrix-assisted laser desorption ionization time-of-flight mass spectrometry coupled with micro-scale derivatization by Chia-Hsien Feng; Hao-Yi Huang; Chi-Yu Lu (pp. 209-214).
Matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS) has been broadly applied to analyze high-molecular-weight compound (such as polymer or proteomic research) but seldom used for low-molecular-weight compound analysis. The objective of this study is the development of a simple analytical method for the determination of the concentration of tripeptide glutathione (GSH) by MALDI-TOF MS. Unfortunately, GSH could not be detected directly by MALDI-TOF MS. Our method is based on the derivatization of GSH with 4-bromomethyl-6,7-dimethoxycoumarin (BrDMC) in acetonitrile using potassium hydroxide (KOH) as a base catalyst. After simple extraction step, the supernatant is spotted on a target plate, mixed with matrix α-cyano-4-hydroxycinnamic acid (CHCA) and then detected by MALDI-TOF MS.Some parameters affecting the derivatization of GSH were investigated, such as the concentration of BrDMC, KOH, different base catalyst, and reaction time, etc. The regression equations of GSH derivative possessed good linearity ( r≧0.995) over the range of 1.0–100.0μM. The relative standard deviation (R.S.D.) and relative error (R.E.) values in intra- and inter-day assays were below 13%, which showed good precision and accuracy. This proposed method was successfully applied to monitor the concentration of GSH in human blood at micro-scale level.

Keywords: Antioxidant; Tripeptide; Derivatization; Micro-scale labelling


Use of a hand-portable gas chromatograph–toroidal ion trap mass spectrometer for self-chemical ionization identification of degradation products related to O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX) by Philip A. Smith; Carmela R. Jackson Lepage; Paul B. Savage; Christopher R. Bowerbank; Edgar D. Lee; Michael J. Lukacs (pp. 215-220).
The chemical warfare agent O-ethyl S-(2-diisopropylaminoethyl) methyl phosphonothiolate (VX) and many related degradation products produce poorly diagnostic electron ionization (EI) mass spectra by transmission quadrupole mass spectrometry. Thus, chemical ionization (CI) is often used for these analytes. In this work, pseudomolecular ([M+H]+) ion formation from self-chemical ionization (self-CI) was examined for four VX degradation products containing the diisopropylamine functional group. A person-portable toroidal ion trap mass spectrometer with a gas chromatographic inlet was used with EI, and both fixed-duration and feedback-controlled ionization time. With feedback-controlled ionization, ion cooling (reaction) times and ion formation target values were varied. Evidence for protonation of analytes was observed under all conditions, except for the largest analyte, bis(diisopropylaminoethyl)disulfide which yielded [M+H]+ ions only with increased fixed ionization or ion cooling times. Analysis of triethylamine- d15 provided evidence that [M+H]+ production was likely due to self-CI. Analysis of a degraded VX sample where lengthened ion storage and feedback-controlled ionization time were used resulted in detection of [M+H]+ ions for VX and several relevant degradation products. Dimer ions were also observed for two phosphonate compounds detected in this sample.

Keywords: Self-chemical ionization; Toroidal ion trap; Chemical warfare agent; Field detection


A novel method of ultrasound-assisted dispersive liquid–liquid microextraction coupled to liquid chromatography–mass spectrometry for the determination of trace organoarsenic compounds in edible oil by Wei-Xun Wang; Tzung-Jie Yang; Zu-Guang Li; Ting-Ting Jong; Maw-Rong Lee (pp. 221-227).
A novel approach, ultrasound-assisted dispersive liquid–liquid microextraction combined with liquid chromatography–mass spectrometry (UA-DLLME with LC–MS) is demonstrated to be quite useful for the determination of trace amounts of organoarsenic compounds in edible oil. The organoarsenic compounds studied include dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and 3-nitro-4-hydroxyphenyl arsenic acid (Roxarsone). Orthogonal array experimental design (OAD) was utilized to investigate the parameter space of conditions for UA-DLLME. The optimum conditions were found to be 4min of ultrasonic extraction using 1.25mL of mixed solvent with 50μL of buffer solution. Under these optimal conditions, the linear range was from 10ngg−1 to 500ngg−1 for DMA and Roxarsone, from 25ngg−1 to 500ngg−1 for MMA. Limits of detection of DMA, MMA and Roxarsone were 1.0ngg−1, 3.0ngg−1 and 5.8ngg−1, respectively. The precisions and recoveries also were investigated by spiking 3-level concentrations in edible oil. The recoveries obtained were over 89.9% with relative standard deviation (RSD) of 9.6%. The new approach was utilized to successfully detect trace amounts of organoarsenic compounds in various edible oil samples.

Keywords: Ultrasound-assisted dispersive liquid–liquid microextraction; Organoarsenicals; Edible oil; Liquid chromatography–mass spectrometry


Detection of counterfeit Scotch whisky samples using mid-infrared spectrometry with an attenuated total reflectance probe incorporating polycrystalline silver halide fibres by Allyson C. McIntyre; Madeleine L. Bilyk; Alison Nordon; Gary Colquhoun; David Littlejohn (pp. 228-233).
Two methods of analysis were developed to permit detection of counterfeit Scotch whisky samples using a novel attenuated total reflectance (ATR) diamond-tipped immersion probe for mid-infrared (MIR) spectrometry. The first method allowed determination of the ethanol concentration (35–45% (v/v)) in situ without dilution of the samples; the results obtained compared well with the supplied concentrations (average relative error of 1.2% and 0.8% for univariate and multivariate partial least squares (PLS) calibration, respectively). The second method involved analysis of dried residues of the whisky samples and caramel solutions on the diamond ATR crystal; principal component analysis (PCA) of the spectra was used to classify the samples and investigate the colorant added. Seventeen test whisky samples were successfully categorised as either authentic or counterfeit in a blind study when both MIR methods were used.

Keywords: Attenuated total reflectance immersion probe; Mid-infrared spectrometry; Polycrystalline silver halide fibres; In situ; analysis; Whisky authentication; Principal component analysis


Determination of trace formaldehyde in blood plasma by resonance fluorescence technology by Yong-Sheng Wang; Xuan Tan; Jin-Hua Xue; Gui-Rong Li; Lin-Fei Shi; Hong-Mei Yang; Lu Liu; Bin Zhou; Xi-Lin Xiao (pp. 234-239).
A novel method for the determination of trace formaldehyde in blood plasma has been established by using resonance fluorimetry technique. It was based on the fact that oxidation of pyronine Y by potassium bromate was catalyzed by formaldehyde in sulfuric acid. When the wavelength interval was at Δ λ=0nm, it was found that the decreased intensity (Δ F) of resonance fluorescence at 574.6nm was proportional to the concentration of formaldehyde in the range of 1.27×10−2 to 2.28μgmL−1. The limit of detection and the average recovery for formaldehyde were 3.80ngmL−1 and 101.6% ( n=6), respectively. The present method had been applied to the determination of trace formaldehyde in blood plasma, and the obtained results were in good agreement with those obtained by the resonance light scattering method.

Keywords: Formaldehyde; Resonance fluorescence; Pyronine Y; Potassium bromate; Blood plasma


Use of the smart tongue to monitor mold growth and discriminate between four mold species grown in liquid media by Guangying Zhao; Xiaona Lin; Wenchao Dou; Shiyi Tian; Shaoping Deng; Jinqin Shi (pp. 240-247).
A novel voltammetric electronic tongue, smart tongue, was employed to monitor the growth of mold and to differentiate between four types of mold grown in liquid medium. Principal component analysis (PCA) was used to extract the relevant information obtained by the smart tongue. Reference growth curves were based on measurements of dry weight and pH. The growth detected by the smart tongue was basically consistent with that observed by the measurement of dry weight and pH. The optimal combinations of electrodes and frequencies for monitoring growth were as follows: for Aspergillus, both the Pt and Au electrodes at 1Hz, 10Hz and 100Hz; for Penicillium, the Pt and W electrodes at 100Hz; for Mucor, the Pt, Pd and W electrodes at the three frequency segments; for Rhizopus, the Pd, Ti and Ag electrodes at the three frequency segments. The Ag electrode at 10Hz or 100Hz frequency could differentiate well between the four types of mold for culturing 6h in the liquid media. Therefore, the smart tongue has a promising future as a modern rapid analytical technology for the real time detection of the growth of mold and for the classification model of mold.

Keywords: Smart tongue; Multifrequency large amplitude pulse voltammetry; Principal component analysis; Liquid culture of mold; Growth of mold


Enzyme-linked immunosensor based on super paramagnetic nanobeads for easy and rapid detection of okadaic acid by Akhtar Hayat; Lise Barthelmebs; Jean-Louis Marty (pp. 248-252).
Okadaic acid (OA), a lipophilic phycotoxin highly toxic to humans is produced by toxigenic dinoflagellates. The need to develop high performing methods for OA analysis able to improve the traditional ones is evident. In this work, competitive indirect enzyme-linked electrochemical immunosensor based on super paramagnetic nanobeads has been developed for the detection of OA. Streptavidin-coated magnetic beads were used as support to immobilize the biotinylated OA. Preliminary, colorimetric tests were performed in order to optimize different experimental parameters. Electrochemical detection was carried out by differential pulse voltammetry (DPV). The limit of detection (LOD) (0.38μgL−1), the mid point value (IC50) (3.15μgL−1) and the time needed (60min) for analysis of a real sample validated the developed electrochemical immunosensor as a promising tool for routine use. The matrix effect and the recovery rate were also assessed, showing an excellent percentage of recovery.

Keywords: Okadaic acid; Immunosensor; Magnetic beads; Differential pulse voltammetry; Mussel


Parallel, fluorous open-tubular chromatography using microstructured fibers by Adam B. Daley; Ramin D. Wright; Richard D. Oleschuk (pp. 253-262).
Although commonly used in gas chromatography, open-tubular columns for liquid chromatography have seen their development hindered by a number of factors both theoretical and practical. Requiring small diameters, great lengths and specialized detection systems to achieve a proper chromatographic response, columns of this sort have largely been ignored despite the highly desirable column performance an optimized system would provide. Here, we introduce the use of microstructured fibers (MSFs) as a platform for the development of multiplexed open-tubular liquid chromatography (OTLC) columns. The multiple, parallel silica channels presented by the MSF act as a promising substrate for an OTLC column, as they have diameters near the ideal range for interactions (1–3μm), minimize flow-induced backpressure through their many uniform paths, and increase the loading capacity compared to a single capillary channel of similar size. Additionally, with outer diameters comparable to regular fused silica capillaries, MSFs can easily be employed in conventional chromatographic systems, eliminating the need for specialized equipment. Finally, MSF columns of this type can be functionalized using silane coupling techniques to allow the introduction of a wide variety of stationary phase chemistries. While in this report we explore the potential and limitations of fluorine-functionalized MSFs as OTLC columns, other stationary phase materials could easily be substituted by choosing appropriate silanization reagents. Particular attention here will be paid to the physical and performance characteristics of the fabricated columns, as well as avenues for their improvement and implementation.

Keywords: Fluorous chemistry; Open-tubular chromatography; Liquid chromatography; Microstructured fiber; Capillary array; Flow profiling


Combining electrophoresis with detection under ultraviolet light and multiple ultrafiltration for isolation of humic fluorescence fractions by Olga E. Trubetskaya; Lubov A. Shaloiko; Dmitrii V. Demin; Victor V. Marchenkov; Ivan I. Proskuryakov; Christian Coelho; Oleg A. Trubetskoj (pp. 263-268).
Polyacrylamide gel electrophoresis of chernozem soil humic acids (HAs) followed by observation under UV (312nm) excitation light reveals new low molecular weight (MW) fluorescent fractions. Ultrafiltration of HAs sample in 7M urea on a membrane of low nominal MW retention (NMWR, 5kDa) was repetitively used for separation of fluorescent and non-fluorescent species. Thirty ultrafiltrates and the final retentate R were obtained. Fluorescence maxima of separate ultrafiltrates were different and non-monotonously changed in the range of 475–505nm. Fluorescence maxima of less than 490nm were detected only in the four first utrafiltrates. For further physical–chemical analyses all utrafiltrates were combined into a fraction called UF<5 (NMW<5kDa). Retentate R demonstrated very weak fluorescence under 270nm excitation, while fluorescence intensity of UF<5 was about six times higher than of the bulk HAs. Fraction UF<5 was further ultrafiltrated on membranes of MNWR 3kDa and 1kDa, yielding three subfractions UF3-5, UF1-3 and UF<1 with NMW 3–5kDa, 1–3kDa and <1kDa, respectively. The validation of the UF procedure was performed by size exclusion chromatography on Sephadex G-25 column. The fluorescence maxima were found to be at 505, 488 and 465nm for UF3-5, UF1-3 and UF<1, respectively, with increasing of fluorescence intensity from UF3-5 to UF1-3 to UF<1 fraction. EPR analysis showed that the amount of free radicals was the largest in retentate R and drastically decreased in fluorescent ultrafiltrates. The results demonstrate that more than one fluorophore is present in chernozem soil HAs complex.

Keywords: Humic acid; Fluorescence; Electrophoresis; Multiple ultrafiltration


Molecularly imprinted solid-phase extraction for determination of tilmicosin in feed using high performance liquid chromatography by Yaqiu Zheng; Yahong Liu; Hongbin Guo; Limin He; Binghu Fang; Zhenling Zeng (pp. 269-274).
A simple, sensitive and reproducible molecularly imprinted solid-phase extraction (MISPE) coupled with high performance liquid chromatographic method was developed for monitoring tilmicosin in feeds. The polymers were prepared using tylosin as mimic template molecule, methacrylic acid as functional monomer and ethylene glycol dimethacrylate as cross-linking monomer, and chloroform as a solvent by bulk polymerization. Under the optimum MISPE conditions, the novel polymer sorbent can selectively extract and enrich tilmicosin from variety of feeds. The MISPE cartridge was better than non-imprinted, C18 and HLB cartridges in terms of both recovery and precision. Mean recoveries of tilmicosin from five kinds of feeds spiked at 1, 10 and 50mgkg−1 ranged from 76.9% to 95.6%, with intra-day and inter-day relative standard deviation less than 7.6%. The linearity was ranged from 1.0 to 100mgL−1 for matrix standard solution ( r=0.9990). The limit of detection was approximately 0.35mgkg−1 and the limit of quantification was approximately 0.98mgkg−1. There was cleaner chromatogram by using MISPE than C18 and HLB SPE.

Keywords: Tilmicosin; Feeds; Molecularly imprinted polymers; Solid-phase extraction; High performance liquid chromatography
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