Moving belt interface with

The full potential of LC-MS could not be exploited until it was possible to study involatile and thermally labile compounds for which electron and chemical ionization are not appropriate. A relatively small number of reports of the use of the moving-belt interface with fast-atom bombardment ionization for the study of these types of compound have appeared. 

Hayes,M. J. Lankmayer,E. P. Vouros,P. Karger,B. L. McGuire, M. 1983. Moving belt interface with spray deposition for liquid chromatogra-phy/mass spectrometry. Anal. Chem., 55,1745-1752. 

He then joined the Central Research Establishment of the Home Office Forensic Science Service (as it then was) at Aldermaston where he developed thermogravimetry-MS, pyrolysis-MS, GC-MS and LC-MS methodologies for the identification of analytes associated with crime investigations. It was here that his interest in LC-MS began with the use of an early moving-belt interface. This interest continued during periods of employment with two manufacturers of LC-MS equipment, namely Kratos and subsequently Interion, the UK arm of the Vestec Corporation of Houston, Texas, the company set up by Marvin Vestal, the primary developer of the thermospray LC-MS interface. 

In summary, it can be said that prior to the development of the thermospray interface there were an increasing nnmber of reports of the analytical application of LC-MS [3] bnt in this present anthor s opinion, based on a nnmber of years of using a moving-belt interface, the technique could not be considered to be routine . The thermospray interface changed this and with the commercial intro-dnction of the combined APCI/electrospray systems in the 1990s the technique, for it now may be considered as a true hybrid technique, has reached maturity (although this should not be taken as a suggestion that there will be no further developments). 

Reference has been made to the problems associated with the presence of highly involatile analytes. Many buffers used in HPLC are inorganic and thus involatile and these tend to compromise the use of the interface, in particular with respect to snagging of the belt in the tunnel seals. The problem of inorganic buffers is not one confined to the moving-belt interface and, unless post-column extraction is to be used, those developing HPLC methods for use with mass spectrometry are advised to utilize relatively volatile buffers, such as ammonium acetate, if at all possible. 

No heat is applied to the interface and it is therefore able to deal with thermally labile materials better than the moving-belt interface. 

Arguably the ultimate LC-MS interface would be one that provides El spectra, i.e. a spectrum from which structural information can be extracted by using famihar methodology, and this was one of the great advantages of the moving-belt interface. There is, however, an incompatibility between the types of compound separated by HPLC and the way in which electron ionization is achieved and therefore such an interface has restricted capability, as previously discussed with respect to the moving-belt interface (see Section 4.2 above). 

Various transport type interfaces, such as SFC-MB-MS and SFC-PB-MS, have been developed. The particle-beam interface eliminates most of the mobile phase using a two-stage momentum separator with the moving-belt interface, the column effluent is deposited on a belt, which is heated to evaporate the mobile phase. These interfaces allow the chromatograph and the mass spectrometer to operate independently. By depositing the analyte on a belt, the flow-rate and composition of the mobile phase can be altered without regard to a deterioration in the system s performance within practical limits. Both El and Cl spectra can be obtained. Moving-belt SFE-SFC-MS" has been described. 

Perhaps the most mechanically complex solution ever developed for uniting HPLC with mass spectrometry was the moving belt interface [54]. The heart of this system was a mechanically driven continuous belt (analogous to an escalator or moving walkway) to which the HPLC eluent was applied. The majority of the mobile phase was evaporated by a heat source (ideally hot enough to vaporize the solvents but not to... 

D.E. Games, P. Hirter, W. Kuhnz, E. Lewis, N.C.A. Weerasinghe and S.A. Westwood, Studies of combined liquid chromatography-mass spectrometry with a moving-belt interface, J. Chromatogr., 203 (1981) 131-138. 

Figure 9. Illustration of the use of extracted ion-current profiles obtained with LC-MS, moving-belt interface, for the detection of carbamate and other pesticides. T op, extracted ion-current profile for 17 major ions second from top, extracted ion-current profile for m/z = 151 to m/z = 181 third from top, extracted ion-current profile for m/z = 86 to m/z = 305 bottom, UV absorption detection at 220 nm. (Reproduced with permission from reference 53. Copyright 1982 Preston Publications.)...

The solvent elimination problem became less of a problem with the commercialization of microbore columns. Hayes et al. (54) studied gradient HPLC-MS using microbore columns and a moving-belt interface. The heart of the system was the spray deposition device designed to be compatible with microbore-column flow rates. Nebulization of the eluent was found to be applicable to a variety of mobile-phase compositions and thus was readily compatible with gradient elution. Figure 13 shows a comparison of UV detection with that obtained with the HPLC-MS system. Applications of this system were demonstrated on water from coal gasification processes. 

Figure 12. Total ion-current profiles obtained with LC-MS, moving-belt interface, for the detection of carbamates and other pesticides. (Reproduced with permission from reference 53. Copyright 1982 Preston Publications.)...

In the moving belt interface, effluent from the column is brought into contact with the belt, and the film of effluent is carried under an infra-red lamp evaporator which rapidly removes most of the solvent. The solute and residual solvent then pass through two vacuum locks, where remaining solvent is removed, and into the ion source of the mass spectrometer where the sample is flash vaporised. The belt then travels over a clean-up heater which removes any residual solute. 

Over 30 years of liquid chromatography-mass spectrometry (LC-MS) research has resulted in a considerable number of different interfaces (Ch. 3.2). A variety of LC-MS interfaces have been proposed and built in the various research laboratories, and some of them have been adapted by instmment manufacturers and became commercially available. With the advent in the early 1990 s of interfaces based on atmospheric-pressure ionization (API), most of these interfaces have become obsolete. However, in order to appreciate LC-MS, one carmot simply ignore these earlier developments. This chapter is devoted to the older LC-MS interfaces, which is certainly important in understanding the histoiy and development of LC-MS. Attention is paid to principles, instrumentation, and application of the capillary inlet, pneumatic vacuum nebulizers, the moving-belt interface, direct liquid introduction, continuous-flow fast-atom bombardment interfaces, thermospray, and the particle-beam interface. More elaborate discussions on these interfaces can be found in previous editions of this book. 

The analysis of steroids is a challenging task. GC-MS has frequently been applied, but requires analyte derivatization [1]. Therefore, over the years most LC-MS interfaces have been tested or applied in the analysis of steroids. As early as 1981, Henion [2] demonstrated the analysis of dexamethasone and cortisone with micro-LC coupled to a capillary-inlet interface. Van der Greef et al. [3] described the quantitation of progesterone in serum using isotope dilution MS in anunonium Cl mode using the moving-belt interface. Henion and coworkers [4] described... 

Figure 1. Schematic diagram of a typical moving belt interface (MBI). [From reference 24 with permission]...

Combined liquid chromatography/mass spectrometry (LC/MS)can play an important role in both qualitative and quantitative bioanalysis. LC/MS can be performed with a number of interfaces. Three interfaces are presently available in our laboratories i.e., the thermospray interface (TSP), the moving-belt interface (MBI), and continuous-flow fast atom bombardment (CF-FAB). These interfaces are supplementary with respect to their applicability and the type of information that can be obtained. 

Nevertheless, Figure 5 demonstrates that the enantiomeric separation using a phosphate buffer in the mobile phase can be coupled via the PSS approach on-line to an LC/MS moving belt interface. Other examples of the PSS approach or similar procedures with other compounds and other LC/MS interfaces have been described (2, 9-14). Besides the actual phase-system switching, which enables the choice of the most favorable solvent for a particular interface, the PSS approach offers some other features as well. The desorption flow-rate used can be adjusted to the capabilities of the LC/MS interface applied. While in the present example with the moving belt a flow-rate of 0.4 ml/min of methanol was used, desorption has also been demonstrated with 1.2 ml/min for a thermospray interfaced),... 

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