Abstract
Liquid–liquid extraction and solid-phase extraction are classical sample preparation techniques that have been used with various types of samples. The fundamentals of these two techniques, as well as several microextraction techniques based on the same principles, are described in this chapter. Application of these techniques to the sample preparation of pharmaceutical dosage forms for analysis is also discussed.
This is a preview of subscription content, log in via an institution to check access.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Abdel-Rehim M (2010) Recent advances in microextraction by packed sorbent for bioanalysis. J Chromatogr A 1217:2569–2580
Akapo S, McCrea CM (2008) SPME-GC determination of potential volatile organic leachables in aqueous-based pharmaceutical formulations packed in overwrapped LDPE vials. J Pharm Biomed Anal 47:526–534
SGE Analytical Science (2010) http://www.sge.com/products/meps
Arthur C, Pawliszyn J (1990) Solid phase microextraction with thermal desorption using fused silica optical fibers. Anal Chem 62:2145–2148
B’Hymer C (2003) Residual solvent testing: a review of gas-chromatographic and alternative techniques. Pharm Res 20:337–344
Baltussen E, Sandra P, David F, Cramers C (1999) Stir bar sorptive extraction (SBSE), a novel extraction technique for aqueous samples: theory and principles. J Microcolumn Sep 11:737–747
Cantwell FF, Losier M (2002) Liquid-liquid extraction (Chapter 11). In: Pawliszyn J (ed) Sampling and sample preparation for field and laboratory. Elsevier, Amsterdam, The Netherlands
Colón I, Richoll SM (2005) Determination of methyl and ethyl esters of methanesulfonic, benzenesulfonic and p-toluenesulfonic acids in active pharmaceutical ingredients by solid-phase microextraction (SPME) coupled to GC/SIM-MS. J Pharm Biomed Anal 39:477–485
Daneshfar A, Khezeli T, Manafi MH (2009) Determination of anti-malaria agent chloroquine using single drop liquid-liquid microextraction. J Sep Sci 32:511–516
Frost RP, Hussain MS, Raghani AR (2003) Determination of pharmaceutical process impurities by solid phase microextraction gas chromatography. J Sep Sci 26:1097–1103
Hennion M-C, Cau-Dit-Coumes C, Pichon V (1998) Trace analysis of polar organic pollutants in aqueous samples. Tools for the rapid prediction and optimization of the solid-phase extraction parameters. J Chromatogr A 823:147–161
Holden AJ (1999) Solvent and membrane extraction in organic analysis (Chapter 2). In: Handley AJ (ed) Extraction methods in organic analysis. Sheffield Academic Press, Sheffield, England
Huidobro AL, Ruperez FJ, Barbas C (2007) Isolation, identification and determination of the major degradation product in alprazolam tablets during their stability assay. J Pharm Biomed Anal 44:404–413
Kataoka H (2005) Recent advances in solid-phase microextraction and related techniques for pharmaceutical and biomedical analysis. Curr Pharm Anal 1:65–84
Kataoka H (2010) Recent developments and applications of microextraction techniques in drug analysis. Anal Bioanal Chem 396:339–364
Kataoka H, Lord HL (2002) Sampling and sample preparation for clinical and pharmaceutical analysis. In: Pawliszyn J (ed) Sampling and sample preparation for field and laboratory, 1st edn. Elsevier Science BV, Amsterdam, The Netherlands
Kenney RR, Forsyth RJ, Jahansouz H (1998) Solid-phase extraction and liquid chromatographic quantitation of the antiarrhythmic drug L-768673 in a microemulsion formulation. J Pharm Biomed Anal 17:679–687
Kolb B, Ettre LS (2006) Static headspace-gas chromatography: theory and practice, 2nd edn. Wiley, Hoboken NJ
Lancas FM, Queiroz MEC, Grossi P, Olivares IRB (2009) Recent development and applications of stir bar sorptive extraction. J Sep Sci 32:813–824
Landis M (2007) The use of mixed-mode ion-exchange solid phase extraction to characterize pharmaceutical drug degradation. J Pharm Biomed Anal 44:1029–1039
Larsen J, Staerk D, Cornett C, Hansen SH, Jaroszewski JW (2009) Identification of reaction products between drug substances and excipients by HPLC-SPE-NMR: ester and amide formation between citric acid 5-aminosalicylic acid. J Pharm Biomed Anal 49:839–842
Lee J, Lee HK, Rasmussen KE, Pedersen-Bjergaard S (2008) Environmental and bioanalytical applications of hollow fiber membrane liquid-phase microextraction: a review. Anal Chim Acta 624:253–268
Ligor M, Buszewski B (1999) Determination of menthol and menthone in food and pharmaceutical products by solid-phase microextraction – gas chromatography. J Chromatogr A 847:161–169
Lokhnauth JK, Snow NH (2005) Determination of parabens in pharmaceutical formulations by solid-phase microextraction – ion mobility spectrometry. Anal Chem 77:5938–5946
Lord H, Pawliszyn J (2000) Microextraction of drugs. J Chromatogr A 902:17–63
Majors R (2002) Sample preparation perspectives: trends in sample preparation. LC GC 29(12):1098–1113
Majors RE (2009) Salting-out liquid-liquid extraction (SALLE). LC GC North America 27(7):526–533
Majors R, Slack G (1997) Sample preparation (Chapter 4). In: Snyder LR, Kirkland JJ, Glajch JL (eds) Practical HPLC method development, 2nd edn. Wiley, New York
Moreno P, Salvado V (2000) Determination of eight water- and fat-soluble vitamins in multi-vitamin pharmaceutical formulations by high-performance liquid chromatography. J Chromatogr A 870:207–215
Nerin C, Salafranca J, Aznar M, Batlle R (2009) Critical review on recent developments in solventless techniques for extraction of analytes. Anal Bioanal Chem 393:809–833
Pan C, Liu F, Ji Q, Wang W, Drinkwater D, Vivilecchia R (2006) The use of LC/MS, GC/MS and LC/NMR hyphenated techniques to identify a drug degradation product in pharmaceutical development. J Pharm Biomed Anal 40:581–590
Pawliszyn J (1997) Solid phase microextraction: theory and practice, 1st edn. Wiley, New York
Pedersen-Bjergaard S, Rasmussen KE (2005) Bioanalysis of drugs by liquid-phase microextraction coupled to separation techniques. J Chromatogr B 817:3–12
Pedersen-Bjergaard S, Rasmussen KE (2008) Liquid-phase microextraction with porous hollow fibers, a miniaturized and highly flexible format for liquid-liquid extraction. J Chromatogr A 1184:132–142
Poole CF (2002) Principles and practice of solid-phase extraction. In: Pawliszyn J (ed) Sampling and sample preparation for field and laboratory, 1st edn. Elsevier Science BV, Amsterdam, The Netherlands
Prieto A, Basauri O, Rodil R, Usobiaga A, Fernandez LA, Etxebarria N, Zuloaga O (2010) Stir-bar sorptive extraction: a view on method optimisation, novel applications, limitations and potential solutions. J Chromatogr A 1217:2642–2666
Rebbeck C, Hammond R, Wong J, Nair L, Raghavan N (2006) Solid-phase extraction and HPLC analysis of methylparaben and propylparaben in a concentrated antibiotic suspension. Drug Dev Ind Pharm 32:1095–1102
USP Reference Tables, Description and Solubility – F (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Reference Tables, Description and Solubility – T (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
Rossi DT, Miller KG (2003) Sample preparation methods for the analysis of pharmaceutical materials (Chapter 8). In: Ahuja S, Alsante KM (eds) Handbook of isolation and characterization of impurities in pharmaceuticals, vol 5. Academic Press/Elsevier, San Diego
Sadek PC (2002) The HPLC solvent guide, 2nd edn. Wiley-Interscience, New York
Sides SL, Polowy KB, Thornquest AD, Burinsky DJ (2001) Identification of a pharmaceutical packaging off-odor using solid-phase microextraction gas chromatography/mass spectrometry. J Pharm Biomed Anal 25:379–386
Slack GC, Snow NH, Kou D (2003) Extraction of volatile organic compounds from solids and liquids (Chapter 4). In: Mitra S (ed) Sample preparation techniques in analytical chemistry. Wiley, Hoboken, NJ
Snow NH, Slack GC (2002) Head-space analysis in modern gas chromatography. Trends Anal Chem 21(9–10):608–617
Supelco Analytical (2010) http://www.sigmaaldrich.com
Thurman EM, Mills MS (1998) Solid-phase extraction: principles and practice. Wiley, New York, NY
USP Monograph for Acetaminophen Suppositories (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Alclometasone Dipropionate Ointment (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Amantadine Hydrochloride Capsules (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Apomorphine Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Carbinoxamine Maleate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Chlordizepoxide Hydrochloride and Clidinium Bromide Capsules (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Chlorothiazide Oral Suspension (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Chlorpromazine Hydrochloride Syrup (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Codeine Phosphate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Codeine Sulfate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Dexamethasone Phosphate Cream (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Dexchlorpheniramine Maleate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Docusate Calcium Capsules (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Docusate Sodium Syrup (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Doxylamine Succinate Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Erythromycin Estolate and Sulfisoxazole Acetyl Oral Suspension (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Flurandrenolide Cream (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Flurandrenolide Ointment (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Guanethidine Monosulfate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Haloperidol Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Hydrocodone Bitartrate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Hyoscyamine Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Levocarnitine Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Mafenide Acetate Cream (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Mebendazole Oral Suspension (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Mesoridazine Besylate Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Mibolerone Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Morphine Sulfate Suppositories (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Neomycin Sulfate Ointment (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Norethindrone Acetate and Ethinyl Estradiol Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Norethindrone Acetate Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Phenmetrazine Hydrochloride Tablets (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Promazine Hydrochloride Syrup (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Simethicone Oral Suspension (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Thioridazine Hydrochloride Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Thioridazine Oral Suspension (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Tolnaftate Cream (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Tolnaftate Gel (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Undecylenic Acid Ointment (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
USP Monograph for Valproic Acid Oral Solution (2010) United States Pharmacopeia, vol 33, reissue. USP-NF Online. http://www.uspnf.com
Wells MJM (2003) Principles of extraction and the extraction of semivolatile organics from liquids (Chapter 2). In: Mitra S (ed) Sample preparation techniques in analytical chemistry. Wiley, Hoboken, NJ
Wille SMR, Lambert WEE (2007) Recent developments in extraction procedures relevant to analytical toxicology. Anal Bioanal Chem 388:1381–1391
Xu L, Basheer C, Lee HK (2007) Developments in single-drop microextraction. J Chromatogr A 1152:184–192
Yamini Y, Reimann CT, Vatanara A, Jönsson JÅ (2006) Extraction and preconcentration of salbutamol and terbutaline from aqueous samples using hollow fiber supported liquid membrane containing anionic carrier. J Chromatogr A 1124(1–2):57–67
Yeung Y-H, Lee T, Grant G, Ma M, Kwong E (2003) A SPME-GC procedure for monitoring peppermint flavor in tablets. J Pharm Biomed Anal 30:1469–1477
Acknowledgments
The authors would like to acknowledge Joanne Lukaszewicz for the development of the LLE sample preparation procedure for Compound A and Sofia Davies, Christophe Chassaing and James Grayson for the development of the LLE sample preparation procedure and LC/MS/MS analysis method for Compound B.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2011 Springer Science+Business Media, LLC
About this chapter
Cite this chapter
Nickerson, B., Colón, I. (2011). Liquid–Liquid and Solid-Phase Extraction Techniques. In: Nickerson, B. (eds) Sample Preparation of Pharmaceutical Dosage Forms. Springer, Boston, MA. https://doi.org/10.1007/978-1-4419-9631-2_4
Download citation
DOI: https://doi.org/10.1007/978-1-4419-9631-2_4
Published:
Publisher Name: Springer, Boston, MA
Print ISBN: 978-1-4419-9630-5
Online ISBN: 978-1-4419-9631-2
eBook Packages: Biomedical and Life SciencesBiomedical and Life Sciences (R0)