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Solid-phase extraction

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sorbents use amine groups which are charged when the pH is below about 9. Strong anion exchange sorbents are useful because any strongly acidic impurities in the sample will bind to the sorbent and usually will not be eluted with the analyte of interest; to recover a strong acid a weak anion exchange cartridge should be used. To elute the analyte from either the strong or weak sorbent, the stationary phase is washed with a solvent that neutralizes the charge of either the analyte, the stationary phase, or both. Once the charge is neutralized, the electrostatic interaction between the analyte and the stationary phase no longer exists and the analyte will elute from the cartridge.
171:. These can be mounted on its specific type of extraction manifold. The manifold allows multiple samples to be processed by holding several SPE media in place and allowing for an equal number of samples to pass through them simultaneously. In a standard cartridge SPE manifold up to 24 cartridges can be mounted in parallel, while a typical disk SPE manifold can accommodate 6 disks. Most SPE manifolds are equipped with a vacuum port, where vacuum can be applied to speed up the extraction process by pulling the liquid sample through the stationary phase. The analytes are collected in sample tubes inside or below the manifold after they pass through the stationary phase. 56:), to separate a mixture into desired and undesired components. The result is that either the desired analytes of interest or undesired impurities in the sample are retained on the stationary phase. The portion that passes through the stationary phase is collected or discarded, depending on whether it contains the desired analytes or undesired impurities. If the portion retained on the stationary phase includes the desired analytes, they can then be removed from the stationary phase for collection in an additional step, in which the stationary phase is rinsed with an appropriate 147:
aliphatic carboxylic acids, which are charged when the pH is above about 5. Strong cation exchange sorbents are useful because any strongly basic impurities in the sample will bind to the sorbent and usually will not be eluted with the analyte of interest; to recover a strong base a weak cation exchange cartridge should be used. To elute the analyte from either the strong or weak sorbent, the stationary phase is washed with a solvent that neutralizes ionic interaction between the analyte and the stationary phase.
45:) is a solid-liquid extractive technique, by which compounds that are dissolved or suspended in a liquid mixture are separated, isolated or purified, from other compounds in this mixture, according to their physical and chemical properties. Analytical laboratories use solid phase extraction to concentrate and purify samples for analysis. Solid phase extraction can be used to isolate analytes of interest from a wide variety of matrices, including urine, blood, water, beverages, soil, and animal tissue. 104:
wet the silica surface. The sample is then added to the cartridge. As the sample passes through the stationary phase, the polar analytes in the sample will interact and retain on the polar sorbent while the solvent, and other non-polar impurities pass through the cartridge. After the sample is loaded, the cartridge is washed with a non-polar solvent to remove further impurities. Then, the analyte is eluted with a polar solvent or a buffer of the appropriate pH.
802: 96: 31: 87:, for each component in the mixture. The chemical considerations for the selection of stationary and mobile phases are similar to those for liquid column chromatography and many of the adsorbents/materials used are the same. The theory, procedures, and aims are different, however, and as an extractive technique it has a unique niche in modern chemical science. 79:, in the sense of having a mobile phase, carrying mixtures through a stationary phase, packed inside a column. The chromatographic process is harnessed to create a solid-liquid extractive technique—allowing separation of a mixture of components by taking advantage of large differences between the solid and liquid phase K 174:
Solid phase extraction cartridges and disks can be purchased with several stationary phases, each of which separates analytes depending on different chemical properties. The basis of most stationary phases is silica that has been bonded to a specific functional group. Some of these functional groups
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Cation exchange sorbents are derivatized with functional groups that interact and retain positively charged cations, such as bases. Strong cation exchange sorbents contain aliphatic sulfonic acid groups that are always negatively charged in aqueous solution, and weak cation exchange sorbents contain
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A typical solid phase extraction involves five basic steps. First, the cartridge is equilibrated with a non-polar or slightly polar solvent, which wets the surface and penetrates the bonded phase. Then water, or buffer of the same composition as the sample, is typically washed through the column to
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It is possible to have an incomplete recovery of the analytes by SPE caused by incomplete extraction or elution. In the case of an incomplete extraction, the analytes do not have enough affinity for the stationary phase and part of them will remain in the permeate. In an incomplete elution, part of
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Anion exchange sorbents are derivatized with positively charged functional groups that interact and retain negatively charged anions, such as acids. Strong anion exchange sorbents contain quaternary ammonium groups that have a permanent positive charge in aqueous solutions, and weak anion exchange
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Reversed phase SPE separates analytes based on their polarity. The stationary phase of a reversed phase SPE cartridge is derivatized with hydrocarbon chains, which retain compounds of mid to low polarity due to the hydrophobic effect. The analyte can be eluted by washing the cartridge with a
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Ion exchange sorbents separate analytes based on electrostatic interactions between the analyte of interest and the positively or negatively charged groups on the stationary phase. For ion exchange to occur, both the stationary phase and sample must be at a pH where both are charged.
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A stationary phase of polar functionally bonded silicas with short carbons chains frequently makes up the solid phase. This stationary phase will adsorb polar molecules which can be collected with a more polar solvent.
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include hydrophobic alkyl or aryl chains chains of variable length (for reversed phase), quaternary ammonium or amino groups (for anion exchange), and aliphatic sulfonic acid or carboxyl groups (for cation exchange).
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A typical solid phase extraction manifold. The cartridges drip into the chamber below, where tubes collect the effluent. A vacuum port with gauge is used to control the vacuum applied to the chamber.
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A stationary phase of silicon with carbon chains is commonly used. Relying on mainly non-polar, hydrophobic interactions, only non-polar or very weakly polar compounds will adsorb to the surface.
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Many of the adsorbents/materials are the same as in chromatographic methods, but SPE is distinctive, with aims separate from chromatography, and so has a unique niche in modern chemical science.
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and non-volatile) from different kinds of media, that can be in liquid or gas phase. The quantity of analyte extracted by the fibre is proportional to its concentration in the sample as long as
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Augusto, Fabio; Hantao, Leandro W.; MogollĂłn, Noroska G.S.; Braga, Soraia C.G.N. (2013). "New materials and trends in sorbents for solid-phase extraction".
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M. Abdel-Rehim, AstraZeneca Application “Syringe for solid phase microextraction”, Current Patents Gazette, week 0310, WO 03019149, p. 77, (2003).
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Hennion, Marie-Claire (1999). "Solid-phase extraction: method development, sorbents, and coupling with liquid chromatography".
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A selection of solid phase extraction cartridges, available in many sizes, shapes, and types of stationary phase.
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E. M. Thurman, M. S. Mills, Solid-Phase Extraction: Principles and Practice, Wiley-Interscience, 1998,
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Raeke, Julia; Lechtenfeld, Oliver J.; Wagner, Martin; Herzsprung, Peter; Reemtsma, Thorsten (2016).
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the analytes remain in the sorbent because the eluent used does not have a strong enough affinity.
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Nigel J.K. Simpson, Solid-Phase Extraction: Principles, Techniques, and Applications, CRC, 2000,
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non-polar solvent, which disrupts the interaction of the analyte and the stationary phase.
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Abdel-Rehim, Mohamed (2011). "Microextraction by packed sorbent (MEPS): A tutorial".
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SPE uses the affinity of solutes, dissolved or suspended in a liquid (known as the
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The stationary phase comes in the form of a packed syringe-shaped cartridge, a
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James S. Fritz, Analytical Solid-Phase Extraction, Wiley-VCH, 1999,
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is reached or, in case of short time pre-equilibrium, with help of
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Buszewski, Boguslaw; Szultka, Malgorzata (July 2012).
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Sample Preparation Techniques in Analytical Chemistry
938: 910: 809: 634: 227:Buszewski, Boguslaw; Szultka, Malgorzata (2012). 445:Environmental Science: Processes & Impacts 360: 358: 356: 354: 352: 350: 348: 612: 8: 27:Process to separate compounds by properties 619: 605: 597: 398:Critical Reviews in Analytical Chemistry 233:Critical Reviews in Analytical Chemistry 219: 194:), which extracts different kinds of 7: 311:TrAC Trends in Analytical Chemistry 25: 161:microextraction by packed sorbent 159:, a 47- or 90-mm flat disk, or a 800: 368:Guide to Solid Phase Extraction 546:. Wiley-Interscience. p.  1: 538:Mitra, Somenath, ed. (2003). 280:10.1016/S0021-9673(99)00832-8 410:10.1080/07373937.2011.645413 245:10.1080/07373937.2011.645413 268:Journal of Chromatography A 184:Solid-phase microextraction 179:Solid-phase microextraction 75:SPE is in fact a method of 988: 837:Electrostatic precipitator 323:10.1016/j.trac.2012.08.012 91:Normal phase SPE procedure 877:Rotary vacuum-drum filter 798: 500:10.1016/j.aca.2011.05.037 920:Aqueous two-phase system 742:Liquid–liquid extraction 817:API oil–water separator 687:Dissolved air flotation 972:Extraction (chemistry) 782:Solid-phase extraction 488:Analytica Chimica Acta 100: 71:SPE and chromatography 39:Solid-phase extraction 35: 18:Solid phase extraction 902:Vacuum ceramic filter 897:Sublimation apparatus 702:Electrochromatography 662:Cross-flow filtration 98: 33: 967:Analytical chemistry 852:Fractionating column 647:Acid–base extraction 628:Separation processes 85:equilibrium constant 672:Cyclonic separation 732:Gravity separation 457:10.1039/C6EM00200E 381:on 13 January 2012 112:Reversed phase SPE 101: 36: 954: 953: 872:Rapid sand filter 767:Recrystallization 747:Electroextraction 707:Electrofiltration 590:978-0-471-24667-1 580:978-0-8247-0021-8 570:978-0-471-61422-7 16:(Redirected from 979: 804: 621: 614: 607: 598: 552: 551: 545: 535: 529: 526: 520: 519: 483: 477: 476: 436: 430: 429: 389: 383: 382: 380: 374:, archived from 373: 365:Supelco (1998), 362: 343: 342: 306: 300: 299: 263: 257: 256: 224: 198:(including both 124:Ion exchange SPE 54:stationary phase 21: 987: 986: 982: 981: 980: 978: 977: 976: 957: 956: 955: 950: 934: 912: 906: 867:Protein skimmer 805: 796: 792:Ultrafiltration 772:Reverse osmosis 752:Microfiltration 727:Froth flotation 667:Crystallization 630: 625: 561: 559:Further reading 556: 555: 537: 536: 532: 527: 523: 485: 484: 480: 438: 437: 433: 391: 390: 386: 378: 371: 364: 363: 346: 308: 307: 303: 265: 264: 260: 226: 225: 221: 216: 181: 153: 144: 142:Cation exchange 135: 126: 114: 93: 82: 73: 28: 23: 22: 15: 12: 11: 5: 985: 983: 975: 974: 969: 959: 958: 952: 951: 949: 948: 946:Unit operation 942: 940: 936: 935: 933: 932: 927: 922: 916: 914: 908: 907: 905: 904: 899: 894: 889: 884: 879: 874: 869: 864: 859: 854: 849: 844: 839: 834: 829: 824: 819: 813: 811: 807: 806: 799: 797: 795: 794: 789: 784: 779: 774: 769: 764: 759: 754: 749: 744: 739: 734: 729: 724: 719: 714: 709: 704: 699: 694: 689: 684: 679: 674: 669: 664: 659: 657:Chromatography 654: 649: 644: 638: 636: 632: 631: 626: 624: 623: 616: 609: 601: 595: 594: 592: 582: 572: 560: 557: 554: 553: 530: 521: 494:(2): 119–128. 478: 451:(7): 918–927. 431: 404:(3): 198–213. 384: 344: 301: 258: 239:(3): 198–213. 218: 217: 215: 212: 210:or agitation. 190:) or a solid ( 180: 177: 152: 149: 143: 140: 134: 133:Anion exchange 131: 125: 122: 113: 110: 92: 89: 80: 77:chromatography 72: 69: 26: 24: 14: 13: 10: 9: 6: 4: 3: 2: 984: 973: 970: 968: 965: 964: 962: 947: 944: 943: 941: 937: 931: 928: 926: 923: 921: 918: 917: 915: 909: 903: 900: 898: 895: 893: 890: 888: 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882:Scrubber 857:Leachate 737:Leaching 682:Dialysis 516:21801877 473:27363664 426:98381163 339:96825406 296:10526783 200:volatile 196:analytes 913:systems 810:Devices 757:Osmosis 192:sorbent 188:polymer 169:syringe 697:Drying 588:  578:  568:  514:  506:  471:  463:  424:  416:  337:  329:  294:  286:  251:  58:eluent 892:Still 422:S2CID 379:(PDF) 372:(PDF) 335:S2CID 83:, or 586:ISBN 576:ISBN 566:ISBN 512:PMID 504:ISSN 469:PMID 461:ISSN 414:ISSN 327:ISSN 292:PMID 284:ISSN 249:ISSN 165:MEPS 548:113 496:doi 492:701 453:doi 406:doi 319:doi 276:doi 272:856 241:doi 60:. 43:SPE 963:: 510:. 502:. 490:. 467:. 459:. 449:18 447:. 443:. 420:. 412:. 402:42 400:. 396:. 347:^ 333:. 325:. 315:43 313:. 290:. 282:. 270:. 247:. 237:42 235:. 231:. 81:eq 620:e 613:t 606:v 550:. 518:. 498:: 475:. 455:: 428:. 408:: 341:. 321:: 298:. 278:: 255:. 243:: 163:( 41:( 20:)

Index

Solid phase extraction

mobile phase
stationary phase
eluent
chromatography
equilibrium constant

96 well plate
syringe
Solid-phase microextraction
polymer
sorbent
analytes
volatile
equilibrium
convection
"Past, Present, and Future of Solid Phase Extraction: A Review"
doi
10.1080/07373937.2011.645413
ISSN
1040-8347
doi
10.1016/S0021-9673(99)00832-8
ISSN
0021-9673
PMID
10526783
doi
10.1016/j.trac.2012.08.012

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