Recent advances in biological sample preparation methods coupled with chromatography, spectrometry and electrochemistry analysis techniques

https://doi.org/10.1016/j.trac.2018.02.005Get rights and content

Highlights

  • A variety of biological samples were described.

  • Recent advances of various biological sample preparation methods were listed.

  • Applications prior to instrumental analysis were summarized.

  • The trends and perspectives of sample preparation methods were proposed.

Abstract

Biological samples are complex and often contain many proteins, lipids and other contaminants, which affect the separation and ionization properties of the analytes. Moreover, the concentration of the analytes is very low in comparison with that of the interfering substances. Therefore, the development of biological sample preparation methods has become more and more challenging. The objective of this review is to provide a broad overview of the main biological samples (urine, blood, plasma, serum, hair, human breast milk, saliva, sweat and skin surface lipids, fecal and tissue), recent advances and applications of various sample preparation methods prior to chromatography, spectrometry and electrochemistry analysis over the past five years. Novel and modern approaches in biological sample preparation are especially emphasized. Finally, challenges and future perspectives to improve development of sample preparation methods are described.

Introduction

The development of biological sample analysis methods has become more and more challenging over the past years due to very demanding requirements in terms of method reliability, sensitivity, speed of analysis and sample throughput. The aim of quantitative analytical method is to provide accurate and reliable determination of the amount of a targeted or untargeted analyte, usually a drug, a metabolite or a biomarker, in complex biological samples. The biological samples usually encompass whole blood, serum, plasma, urine, saliva, breast milk, sweat, cerebrospinal fluid, gastric fluid, exhaled breath, and tissue samples (i.e., hair, nail, skin, bone, muscle) [1], cells, cell culture, culture media and so on. Types of biological samples used in CE-MS metabolomics studies were listed [2]. Except tissue and cell, urine and serum are the most often used samples. However, matrix effects, such as the presence of endogenous or exogenous macromolecules, small molecules and salts which interfere with analysis, low analyte concentration and biological matrix that are incompatible with instrument, all necessitate sample preparation before analysis [3]. Therefore, sample preparation starting from enhancement of selectivity and sensitivity of the analysis to improving analytical criteria and/or protecting the analytical instrument from possible damage might be employed. Sample preparation is of utmost importance for obtaining the analytes of interest in a suitable injection solution able to provide reliable and accurate results. It has substantial objectives before sample injection, including [4]:

  • 1.

    reducing or eliminating matrix interferences or undesired endogenous compounds;

  • 2.

    increasing selectivity for targeted analyte(s);

  • 3.

    preconcentrating the sample to enhance sensitivity; and

  • 4.

    stabilizing the sample by reconstituting it in an inert solvent.

A number of research efforts dealing with biological sample preparation methods have been reported. There are also some valuable reviews about biological sample preparation.

Soltani et al. [3] and Namera [5] gave reviews focused on the achievements in the pretreatment of biological samples and investigated sample pretreatments in six categories (i.e., dilution, filtration/dialysis, precipitation, extraction (solid-phase extraction, liquid liquid extraction]), novel techniques (turbulent flow chromatography, immunoaffinity method, electromembrane extraction) and combined methods.

Nováková [6] reviewed some traditional biological sample preparation techniques, such as solid phase extraction (SPE), liquid liquid extraction (LLE), protein precipitation (PP), and modern biological sample preparation techniques such as solid phase microextraction (SPME), stir-bar sorptive extraction (SBSE), microextraction by packed sorbent (MEPS), disposable pipette tips extraction (DPX), single drop microextraction (SDME), hollow-fiber liquid phase microextraction (HF-LPME), dispersive liquid-liquid microextraction (DLLME) and dried blood spot (DBS) prior to liquid chromatography-mass spectrometry method (LC-MS).

Lum et al. [7] discussed four aspects of the recent development in metal preconcentration methods in clinical samples, namely the use of ionic liquids (ILs) in DLLME and SDME extraction, sorption by nanomaterials in SPE, preconcentration using surfactants in CPE and liquid phase extraction, and automation (on-line SPE and DLLME). Delafiori et al. [8] introduced some sample preparation methods of arsenic (As), selenium (Se) and mercury (Hg) elements in various clinical matrices.

Fernández-Peralbo and Luque de Castro [9] presented an overview of researches on preparation of urine samples prior to targeted or untargeted metabolomics mass-spectrometry analysis.

Oh and Lee [10] described sample preparation methods such as PP, LLE and SPE for liquid chromatographic analysis of phytochemicals in biological fluids.

An important bottleneck of biological sample preparation is the presence of matrix effects, which have recently received lots of attention. Biological matrices are complex and often contain proteins, lipids, drugs, salts, acids, bases and various other organic and inorganic compounds with similar properties to the analytes, which may interfere with the analytes measurement. Therefore, sample preparation is a very vital part prior to the instrument analysis. However, sample preparation step still remains the most time-consuming and labor-intensive step of biological analysis. An important trend shared by the fundamental researches on the above sample preparation techniques relates to the development of more accurate, precise, selective and robust preparation methods. It has become a hot issue to new sorbents, on/in-line sample preparation methods coupled with chromatography, spectrometry and electrochemistry analysis. In this review, we therefore summarized some biological samples such as urine, blood, plasma, serum, hair, human breast milk, saliva, sweat and skin surface lipids, fecal, some tissue samples and so on, highlighted sample preparation techniques of these samples. We provided an updated, essential summary of the most important sample preparation methods coupled with chromatography, spectrometry and electrochemistry analysis for biological samples. We also discussed the present limitations and expected future trends of biological sample preparation methods for better advancement. There is no restrict definition of sample pretreatment and preparation in the published researches. Some may consider both steps as a single step, they called them sample preparation. In this review, the former step, consisting of sampling time and collection, preservative addition, volume correction, pH adjustment, dilution, enzymatic hydrolysis and so on, is called sample pretreatment; the following step, consisting of PP, LLE, SPE, SPME, LPME and so on, is called sample preparation.

Section snippets

Urine

Urine is composed of over 95% water, plus sodium, ammonia, phosphate, sulfate, urea, creatinine, proteins and products processed by the kidney and liver, including drugs and metabolites [9]. Urine is slightly acid in the morning (pH = 6.5–7.0), generally becoming more alkaline (pH = 7.5–8.0) by evening in healthy people primarily because no food or beverages are consumed while sleeping. As a sample for analysis, it has its own advantages compared with serum:

  • (1)

    can be obtained in large volume by

Sample preparation

Related description about liquid and solid phase extraction such as LLE, LPME (DLLME, SDME, HF-LPME and etc.), SPE, SPME, stir-bar sorptive extraction (SBSE), and matrix solid phase dispersion (MSPD) is presented in our previous review [39], [40]. Also, these methods used for biological samples are reviewed in detail by other research groups [3], [5], [6], [7], [9], [10], [41], [42], [43], [44]. Sample preparation methods applied in bioanalytical sample and their important features including

Applications

In order to obtain high sensitive results of analytes and protect the analytical instrument (including chromatography, spectrometry and electrochemical instrument), sample pretreatment/preparation must be an important part of the whole analysis. Below, we provide an elaborated update on the simple introduction of these sample preparation methods application.

Conclusions and perspectives

This review of sample preparation for biological samples coupled with chromatography, spectrometry and electrochemistry technique includes an enormous variety of methods (LLE, LPME, LLLME, DLLME, CPE, SPE, SPME, SBSE and so on). Undoubtedly, the sample preparation/pretreatment of biological samples is an important bottleneck of bioanalytical methods and has become a hot topic in analysis. Important features of some solid and liquid extraction methods, such as extraction time, solvent volume,

Acknowledgements

Financial support from the National Natural Science Foundation of China (No. 81660355, 81460328, 41676141), and Training Foundation of Hainan Medical University (No. HY2013-04, HY2013-16) are gratefully acknowledged.

References (272)

  • S.H. Mathes et al.

    The use of skin models in drug development

    Adv. Drug Deliv. Rev.

    (2014)
  • J.Y. Wan et al.

    Biotransformation and metabolic profile of American ginseng saponins with human intestinal microflora by liquid chromatography quadrupole time-of-flight mass spectrometry

    J. Chromatogr. A

    (2013)
  • Á. Ríos et al.

    Sample preparation for micro total analytical systems (μ-TASs)

    TrAC Trend. Anal. Chem.

    (2013)
  • Y. Wen et al.

    Recent advances in solid-phase sorbents for sample preparation prior to chromatographic analysis

    TrAC Trend. Anal. Chem.

    (2014)
  • A. Chisvert et al.

    An overview of the analytical methods for the determination of organic ultraviolet filters in biological fluids and tissues

    Anal. Chim. Acta

    (2012)
  • R.A. Biddlecombe et al.

    Automated protein precipitation by filtration in the 96-well format

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (1999)
  • J. Ma et al.

    A fully automated plasma protein precipitation sample preparation method for LC-MS/MS bioanalysis

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2008)
  • C. Ji et al.

    Simultaneous determination of plasma epinephrine and norepinephrine using an integrated strategy of a fully automated protein precipitation technique, reductive ethylation labeling and UPLC-MS/MS

    Anal. Chim. Acta

    (2010)
  • C. Kitchen

    A semi-automated 96-well protein precipitation method for the determination of montelukast in human plasma using high performance liquid chromatography/fluorescence detection

    J. Pharmaceut. Biomed.

    (2003)
  • A. Jain et al.

    Salting-out assisted liquid-liquid extraction for the determination of biogenic amines in fruit juices and alcoholic beverages after derivatization with 1-naphthylisothiocyanate and high performance liquid chromatography

    J. Chromatogr. A

    (2015)
  • Y. Wen et al.

    Salting-out assisted liquid-liquid extraction with the aid of experimental design for determination of benzimidazole fungicides in high salinity samples by high-performance liquid chromatography

    Talanta

    (2013)
  • I.M. Valente et al.

    Another glimpse over the salting-out assisted liquid-liquid extraction in acetonitrile/water mixtures

    J. Chromatogr.

    (2013)
  • W. Wei et al.

    pH-mediated dual-cloud point extraction as a preconcentration and clean-up technique for capillary electrophoresis determination of phenol and m-nitrophenol

    J. Chromatogr. A

    (2008)
  • C. Nong et al.

    Dual-cloud point extraction coupled to high performance liquid chromatography for simultaneous determination of trace sulfonamide antimicrobials in urine and water samples

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2017)
  • S.S. Arain et al.

    Preconcentration of toxic elements in artificial saliva extract of different smokeless tobacco products by dual-cloud point extraction

    Microchem. J.

    (2014)
  • S.A. Arain et al.

    Application of dual-cloud point extraction for the trace levels of copper in serum of different viral hepatitis patients by flame atomic absorption spectrometry: a multivariate study

    Spectrochim. Acta Mol. Biomol. Spectrosc.

    (2014)
  • M. Rezaee et al.

    Determination of organic compounds in water using dispersive liquid-liquid microextraction

    J. Chromatogr. A

    (2006)
  • M.S. El-Shahawi et al.

    Dispersive liquid-liquid microextraction for chemical speciation and determination of ultra-trace concentrations of metal ions

    TrAC Trend. Anal. Chem.

    (2013)
  • M.I. Leong et al.

    Dispersive liquid-liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron-capture or mass spectrometry detection

    J. Chromatogr. A

    (2008)
  • L.E. Vera-Avila et al.

    Capabilities and limitations of dispersive liquid-liquid microextraction with solidification of floating organic drop for the extraction of organic pollutants from water samples

    Anal. Chim. Acta

    (2013)
  • M.R. Khalili Zanjani et al.

    A new liquid-phase microextraction method based on solidification of floating organic drop

    Anal. Chim. Acta

    (2007)
  • H. Yan et al.

    Recent development and applications of dispersive liquid-liquid microextraction

    J. Chromatogr. A

    (2013)
  • N.M. Kocherginsky et al.

    Recent advances in supported liquid membrane technology

    Sep. Purif. Technol.

    (2007)
  • G. Zhao et al.

    Determination of short-chain fatty acids in serum by hollow fiber supported liquid membrane extraction coupled with gas chromatography

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2007)
  • S. Pedersen-Bjergaard et al.

    Electrokinetic migration across artificial liquid membranes. New concept for rapid sample preparation of biological fluids

    J. Chromatogr. A

    (2006)
  • C. Basheer et al.

    Simultaneous extraction of acidic and basic drugs at neutral sample pH: a novel electro-mediated microextraction approach

    J. Chromatogr. A

    (2010)
  • H. Lord et al.

    Evolution of solid-phase microextraction technology

    J. Chromatogr. A

    (2000)
  • A. Namera et al.

    Extraction of amphetamines and methylenedioxyamphetamines from urine using a monolithic silica disk-packed spin column and high-performance liquid chromatography-diode array detection

    J. Chromatogr. A

    (2008)
  • T. Saito et al.

    Simultaneous determination of amitraz and its metabolite in human serum by monolithic silica spin column extraction and liquid chromatography-mass spectrometry

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2008)
  • A. Dupuy et al.

    Simultaneous quantitative profiling of 20 isoprostanoids from omega-3 and omega-6 polyunsaturated fatty acids by LC-MS/MS in various biological samples

    Anal. Chim. Acta

    (2016)
  • C. Gong et al.

    Post-pellet-digestion precipitation and solid phase extraction: a practical and efficient workflow to extract surrogate peptides for ultra-high performance liquid chromatography–tandem mass spectrometry bioanalysis of a therapeutic antibody in the low ng/mL range

    J. Chromatogr. A

    (2015)
  • M. Mazzarino et al.

    A liquid chromatography-mass spectrometry method based on class characteristic fragmentation pathways to detect the class of indole-derivative synthetic cannabinoids in biological samples

    Anal. Chim. Acta

    (2014)
  • Y. Cao et al.

    Quantification of levornidazole and its metabolites in human plasma and urine by ultra-performance liquid chromatography-mass spectrometry

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2014)
  • Y. Chang et al.

    Analysis of bisphenol A diglycidyl ether (BADGE) and its hydrolytic metabolites in biological specimens by high-performance liquid chromatography and tandem mass spectrometry

    J. Chromatogr. B Analyt. Technol. Biomed. Life Sci.

    (2014)
  • L. Zuluaga-Idarraga et al.

    Validation of a method for the simultaneous quantification of chloroquine, desethylchloroquine and primaquine in plasma by HPLC-DAD

    J. Pharm. Biomed. Anal.

    (2014)
  • J.A. Kiebooms et al.

    Validated ultra high performance liquid chromatography-tandem mass spectrometry method for quantitative analysis of total and free thyroid hormones in bovine serum

    J. Chromatogr. A

    (2014)
  • L. Ren et al.

    Study on pharmacokinetic and tissue distribution of lycorine in mice plasma and tissues by liquid chromatography-mass spectrometry

    Talanta

    (2014)
  • X.M. Zhuang et al.

    Simultaneous determination of triptolide and its prodrug MC002 in dog blood by LC-MS/MS and its application in pharmacokinetic studies

    J. Ethnopharmacol.

    (2013)
  • S. Rocchi et al.

    Quantitative profiling of retinyl esters in milk from different ruminant species by using high performance liquid chromatography-diode array detection-tandem mass spectrometry

    Food Chem.

    (2016)
  • Y.J. Xue et al.

    Bioanalysis of drug in tissue: current status and challenges

    Bioanalysis

    (2012)
  • Cited by (0)

    View full text