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Postpuri cation analytical SFC/MS/NCD is used as ell to validate puri ed samples Our group also has custom modi ed19 a Berger Instruments preparative SFC for use in support of the puri cation20,21 of libraries synthesized by the high-throughput organic synthesis group and have integrated this system into the existing preparative HPLC puri cation processes Speci cs of this instrument and applications to the puri cation of libraries will be detailed within the text of this chapter MW-triggered fraction collection in SFC has been reported by the Dupont group,22 whose system is comprised of a Gilson (Middletown, WI) semipreparative SFC and autosampler and a PE Sciex (Foster City, CA) mass spectrometer with ESI source, operated in the positive ion mode.

A simple foil seal is placed over the collection tubes to improve recovery into the fraction collection system, and provide a loose barrier that encourages retention of the methanol portion of the eluant and departure of the carbon dioxide Two solvent makeup pumps were added to the system: one to provide additional ow to the fraction collector as carbon dioxide departs and a second to provide auxiliary ow of methanol containing formic acid additive to the mass spectrometer stream in order to dilute sample concentration as well as to improve ion signal and peak shape Fraction collection is triggered when signal for a component of the desired molecular weight from each sample goes above a pre-set threshold value and is controlled through the mass spectrometer software package.

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This system is capable of purifying crude samples up to 50 mg in weight for chromatographically well-behaved samples, and it is used by DuPont scientists for chiral separations as well as general library puri cations Kassel from the DuPont group has also reported23 preliminary efforts toward a MWtriggered preparative SFC system on the Berger platform Ontogen researchers24,25 have custom designed a MW-triggered semipreparative SFC system for puri cation of their parallel synthesis libraries This parallel four-channel system is capable of processing four microtiter format plates simultaneously A protocol is used whereby UV detection is rst employed to identify peaks from each sample as they elute, followed by diversion of a split stream from the eluant to a mass spectrometer for molecular weight determination.

Each of the four SFC columns is monitored by a dedicated UV detector, but as peaks are identi ed by their respective detectors, all are diverted to a single time-of- ight mass spectrometer Fraction collection is initiated by the mass spectrometer, which identi es the desired target peak and then triggers fraction collection into a target plate In addition to collection of the desired component, reaction by-products are diverted into an ancillary plate whose fraction collection is initiated by identi cation by the mass spectrometer of a MW other Bar Code In NET Using Barcode printer for NET Related: Excel QR Code Generating , Generate UPC-E Excel , Generate Code 39 Java.

MS radio access capability this parameter contains various indicators related to radio signalling capabilities of the MS Examples include upported access technologies and transmission power capabilities The inclusion of the IMEI in CAP IDP-GPRS is done in a backwards-compatible manner The IMEI is placed after the ellipsis in the argument of CAP IDP-GPRS As a result, the same CAP application context may be used for GPRS control in CAMEL phase 4 A further result is that no new version of GPRS-CSI is de ned in CAMEL phase 4; the GPRS-CSI in CAMEL phase 4 still indicates CAMEL capability handling = CAP v3 If an SCP does not support the reported IMEI in IDP-GPRS, then that SCP will ignore that parameter, if received. UPC A Drawer In .NET Framework Using Barcode printer for .NET framework .Related: Generate Code 39 C# , Interleaved 2 of 5 Generating VB.NET , Print Intelligent Mail Excel

tion for each of the puri cation chemists in HTP in a custom software package henever possible, samples from multiple sources are grouped for puri cation This can be done whenever the optimal wavelength for fraction collection trigger and the optimal gradient elution method are deemed identical for multiple sample sets Doing so increases ef ciency of the overall process The software allows the assignment of puri cation parameters to a speci c preparative scale HPLC Upon completion of puri cation, data les and fraction collection racks are passed on for loop injection MS of fractions selected by the puri cation chemist This system of UVtriggered fraction collection followed by MS validation has been the mainstay puri cation technique for HTP at Abbott for several years.

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It was adopted on the principle that several relatively inexpensive yet slow HPLCs feeding into a single more costly but fast MS give good value and allow for expansion We have thus succeeded in accommodating initially two and presently four preparative UV/ELSD-triggered HPLCs At this point custom software allows importation of chromatograms and correlated mass spectrometry data to be reviewed by the puri cation chemist (as shown in Figure 112) Those fractions corresponding to the desired component(s) are selected for sample labeling and dry-down The sample, along with a Puri cation Report (as shown in Figure 113), is returned to the submitting chemist HPLC (MS) In addition to the UV or ELSD triggered HPLC instruments described above, an MW-triggered HPLC instrument is available in our HTP facility.

This is commercially known as the Agilent (Wilmington, DE) 1100 series LC/MSD, which includes a PDA detector and mass spectrometer and a Gilson 215 liquid-handler for injection and fraction collection An Antek (Houston, TX) 8060 nitrogen speci c detector (Chemiluminescent Nitrogen Detection CLND) was integrated into the system in order to achieve on-line determinations of sample weights during puri cation Custom macros as well as a custom data browser were written for sample tracking and data viewing,27 which includes CLND quantitation information made available in the nal client report The chromatography column employed on this system is a Phenomenex LunaR C8, 5-m particle size column of 50 212 mm dimensions, used for the puri cation of 10 to 50 mg HTOS libraries Standard gradient elution methods used are 0 100% MeOH : 01% aqueous TFA, 10 100% MeOH : 01% aqueous TFA, 20 100% MeOH : 0.

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