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Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in the Clinical Laboratory*

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Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in the Clinical Laboratory* ANNALS OF CLINICAL AND LABORATORY SCIENCE, Vol. 25, No. 3 Copyright © 1995, Institute for Clinical Science, Inc. Inductively Coupled Plasma Mass Spectrometry for Trace Element Analysis in the Clinical Laboratory* KERN L. NUTTALL, M.D., Ph.D., WILLIAM H. GORDON, CLS (NCS), and K. OWEN ASH, Ph.D. Department of Pathology, University of Utah School of Medicine, Salt Lake City, UT 84108 ABSTRACT Inductively coupled plasma mass spectrometry (ICP-MS) is a relatively new technique for trace element analysis. The basic operating principles of ICP-MS are described and our experience with this technique in a clinical setting is discussed for the analysis of serum, whole blood, and urine. Advantages to ICP-MS include the favorable detection limits (0.01 to 0.1 |xg/L for many elements), simple specimen preparation, high throughput (about 40 specimens per hour), and the ability to measure more than one element simultaneously. A major disadvantage is the high capital cost of the instrumentation. Heavier elements, such as lead, are well-suited for ICP-MS analysis, whereas lighter elements are prone to more interfer­ ences. Lighter elements which are not amenable to assay by ICP-MS include chromium and iron. The ability to measure isotopes is a major advantage for mass spectrometry methods and has the potential to expand the usefulness of trace element analysis. Introduction powerful technique is now beginning to find acceptance for analysis of clinical This article is intended to introduce specimens. Our experiences are laboratorians to the potential of induc­ described with ICP-MS for analysis of tively coupled plasma mass spectrometry trace elements which began in 1989 (ICP-MS) as an emerging technology for when methods for commercial instru­ analysis of trace elements in biological ments! were developed for analysis of specimens. Until recently, ICP-MS has trace elements in biological specimens, been primarily used in the environmen­ primarily urine, serum and whole blood. tal field for analysis of water and air. This The basic operating principles are described and both the advantages and limitations to ICP-MS are discussed. * Send reprint requests to: Kern L. Nuttall, M.D., Ph.D., Department of Pathology, University of Utah School of Medicine, % ARUP—500 Chipeta Way, t Perkin-Elemer Elan 500 and, subsequently, Salt Lake City, UT 84108. Elan 5000. 264 0091-7370/95/0500-0264 $01.20 © Institute for Clinical Science, Inc. INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR TRACE ELEMENT ANALYSIS 265 The ICP-MS Instrument men is lost to the drain of the spray cham­ ber. More efficient direct injection sys­ Inductively coupled plasma mass spec­ tems are available,3 but have not to date trometry is a relatively new technique. been implemented in our laboratory. The first analytical mass spectra were Direct injection into the plasma has the obtained from an ICP in 1978, and the potential to increase the throughput sig­ first commercial instruments were intro­ nificantly and decrease the specimen vol­ duced by Sciex in 1983.1 A typical instru­ ume required for analysis. ment (figure 1) consists of an ICP torch A typical ICP torch consists of three connected via an interface to a mass spec­ concentric quartz tubes and a coil which trometer. The sample solution to be ana­ carries high-energy radiofrequency lyzed is transferred by a peristaltic pump power in the range of 1 to 3 kilowatts. to a nebulizer which converts the solu­ The radiofrequency power acts on the tion into an aerosol. The aerosol is car­ argon exiting the middle tube to produce ried by argon gas into the center of the a plasma of more than 6000°K. The ICP torch. The high temperature plasma plasma is created by the energetic colli­ vaporizes and ionizes the sample, and sions among the argon atoms oscillating directs ions into the mass spectrometer, in the high-energy radiofrequency field. where the elements of interest are The outer tube carries argon gas which detected on the basis of the mass- flows at a high rate to act as a barrier or to-charge (m/z) ratio. A major disadvan­ coolant layer to prevent the torch from tage to ICP-MS is the high capital melting in the intense heat of the plasma. cost, although recently introduced The inner tube carries the aerosolized benchtop instruments are considerably sample into the center of the plasma. less expensive .2 Specimens introduced into the plasma A nebulizer is an easy and inexpensive are rapidly vaporized, atomized, and ion­ way to introduce a sample solution into ized. The flow rate of the argon carrier the ICP torch. Our instruments use gas positions the plasma for sampling Meinhard-type nebulizers made of boro- into the mass spectrometer. silicate glass, which produce an aerosol The ICP torch can also be coupled to when the argon carrier gas is forced an atomic emission spectrometer (ICP- through a small capillary into a spray AEM), which uses photon emission to chamber. One problem with this design detect trace elements. While ICP-AEM is that more than 95 percent of the speci­ instruments are less expensive, they may ICP Torch Interface Mass Spectrometer Nebulizer Quadrupole F ig u r e 1. Schematic of a typical instrument for inductively coupled plas­ mas spectrometry. The inductively coupled plasma (ICP) torch, which operates at atmo­ spheric pressure, is cou­ pled to the mass spec­ -Argon Sample *” Gas trometer through an Solution interface. RF Power IVacuuml I Vacuum] Supply 1 Pump 1 1 Pump 1 Computer 266 NUTTALL, GORDON, AND ASH also suffer from greater interferences and mined by the ability of the Channeltron do not have the low detection limits electron multiplier to handle intense ion of ICP-M S.3 beams and is about six orders of magni­ The ICP-MS interface must transfer tude above the detection limit, thereby ions from the torch at several thousand providing a wide usable range for most degrees Kelvin and atmospheric pressure trace elements. The mass resolution and into a mass spectrometer which operates computer capabilities of the ICP-MS in a vacuum at low temperature. The first often permit multiple trace elements to stage of the interface consists of a sam­ be analyzed at the same time, thereby pler cone with an orifice of about 0.5 mm significantly increasing efficiency in the positioned to collect ions from the laboratory.4 For example, in our labora­ plasma. Because of the intense heat gen­ tory assays for arsenic, cadmium, anti­ erated by the torch, the sampler cone mony, tellurium, thallium, lead, and bis­ must be cooled in an efficient manner muth are conducted at the same time. with refrigerated water. The sampler The ICP-MS instruments often achieve cone opens into an interface region, a signal stability of about ± 5 percent rela­ which is pumped down to approximately tive standard deviation over several 1 torr by a mechanical pump. The second hours, and an internal standard can stage of the interface is the skimmer improve this to about 1 percent. Prob­ cone, which is placed several millimeters lems with instrumental drift can occur behind the sampler orifice. The orifice of with specimens containing high concen­ the skimmer cone opens directly into the trations of salts which can deposit on the vacuum chamber of the mass spectrome­ sampler and skimmer cones. To monitor ter. A quadrupole mass filter is usually drift, control material is run every 15 used to provide low-cost mass discrimi­ specimens; when the control falls out of nation. (More costly high-resolution mass range, the instrument is recalibrated. spectrometers can circumvent many of Assays for heavy elements, such as lead, the isobaric overlaps that occur with quad- tend to be remarkably stable and seldom rupoles). Ions exiting the quadrupole require recalibration, whereas lighter are detected by a Channeltron electron elements such as aluminum require con­ multiplier (CEM). siderably more frequent recalibration. Approximately 40 patient specimens can Performance Characteristics be processed per hour with the major determinant of throughput being the Over 50 elements have detection limits time required to pump a specimen in the range of 0.01 to 0.1 (xg/L, often through the nebulizer and into the torch. matching or surpassing those of atomic In general, the instruments have been absorption spectrometry .3 Only eight ele­ easy to maintain. Routine maintenance ments (carbon, nitrogen, oxygen, fluo­ requires approximately 1 0 to 2 0 m in per rine, silicon, phosphorus, sulfur, and day and consists primarily of cleaning the chlorine) have detection limits greater torch and sampler cone. Minor problems than 10 (Jig/L owing to their low degree of consist of items such as breaking of the ionization in the plasma torch. Detection torch during cleaning. Twice a year the limits are usually defined as three stan­ manufacturer schedules preventative dard deviations above the mean of the maintenance, which usually requires a blank and are determined under ideal full day off-line. With instruments less conditions. Practical detection limits are than three years old, approximately one often an order of magnitude poorer. The major failure per instrument/year has upper limit of the linear range is deter­ occurred where downtime lasted 3 to 7 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY FOR TRACE ELEMENT ANALYSIS 267 days. Our older instrument (Elan 500) is Interferences now suffering more frequent failures. Unavailability of parts has been the chief Because a mass spectrometer discrimi­ factor in the length of downtime. nates on the basis of the mass-to-charge ratio, interferences in ICP-MS come pri­ Specimen Preparation marily through mass overlap from: (1 ) Specimen preparation typically con­ polyatomic ions, (2 ) elements with the sists of diluting or digesting the speci­ same isotopic masses (elemental isobaric men in mineral acids and analyzing the overlap), and (3) doublely charged ions.
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