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www.promochrom.cominfo@promochrom.com Integration of SPE with LC and LC-MS analysis Haibin WanPromoChrom Technologies Ltd. Integration of sample cleanup with instrumental analysis helps to improvedata reproducibility and increase sample throughput. It can also releasechemists from labor intensive routines. PromoChrom developed twosolutions for the integration. Solution 1： SPE-04 multi functional SPE The instrument can perform both online and offline SPE. In addition， it has afunction for online derivatization at controlled temperature after columncleanup (between column derivatization). 8 6 Syringe pump 1 heater Wash Change a Condition Load needle new SPE with 1 or 2 sample cartridge solvents 具 Typical Collect fraction Elute with working (Offline SPE) 1-2 solvents 具 Inject to HPLC Derivatize with 1 or 2 Collect fraction trigger to start reagents at controlled (Online SPE) HPLC temperature (Optional) Application example： Analysis of hormones in milk powder 1.Extract estrone from milk powder using acetonitrile 2.Load extracts to SAX SPE column 3.Derivatize the collected fraction 4.Inject into HPLC 5.HPLC analysis using a C18 column for separation and UV detection at360 nm. Features of SPE-04 1. Offline SPE It can work for offline column cleanup and fraction collection. Whenworking in offline mode， computer is not necessary. Users can set up theinstrument quickly using the 7 buttons. Easy operation. The offline modedoes not need computer. 2. Online SPE In online mode， the collected fraction is directly injected into an HPLC orLC-MS for final determination. The control software for online SPE is userfriendly and is compatible with most HPLC software. 3. Direct sample injection SPE-04 can work as an auto sampler. Therefore， the HPLC does not needto have another sample introduction device. 4. Derivatization after cleanup and at controlled temperature Conventional pre column derivatization is normally carried out at ambienttemperature. The reaction temperature limits the selection ofderivatization reagents. Besides， the sample matrix may interfere thereaction if a cleanup has not been performed. By providing cleanupbefore derivatization and a well controlled temperature， SPE-04 givesmore reliable derivatization results. Solution 2： LC-03 online SPE for Direct Analysis of Liquid Samples LC-03 online SPE uses valves and a syringe pump to transfer sample toSPE column and then to the HPLC system. The control software looks Users only need to select thenecessary actions. Such as “loadsample"，“add reagent 1”，“inject”，“start LC"， etc. Part from online SPE 1. Draw sample or elution solvent Part from online SPE 3. Wash SPE column in normal direction toremove interference and small particles 2. Load sample to SPE column in reversed direction 4. Elute trapped analytes to HPLC column XQ Ptenanthvore 5 pob， inject 40mL一 200 150 109 Direct analysis of phenanthrene in tap water at 5 ppb and 50 ppt level using online SPE coupled withHPLC. SPE column， TrapN； analytical column PromSil C18； sample volume， 40 mL； flow rate forsample loading， 6 mL/min； detection wavelength， 252 nm. Features of LC-03 1. Allow elution of SPE column in two directions It helps to prevent trapped particle from entering analytical column and obtain anarrow band when eluting the trapped analytes from SPE column to HPLCcolumn. 2. Standalone operation The device can be controlled using built-in methods for most applications. It iseasy to hook up to any LC or LC-MS system without disturbing the computerenvironment. Comparison of the two online SPE solutions： SPE-04 LC-03 Use ofSPE column One SPE column for each sample.More tolerant to dirty samples. Widerselection of suitable SPE columns. One SPE column for multiple samples(50-100). Less selection of SPE columns dueto mobile phase compatibility issue. More suitable for clean samples. Use of sample Trapped analytes are washed to avial and then loaded to injection loop.Only a portion is used for analysis Trapped analytes are directly introduced toHPLC column. 100% of trapped analytesare analyzed. Number of samples Up to 41 samples per batch Up to 10 samples per batch Volume ofsamples Up to 20 mL Up to 100 mL Use high performance SPE column to improve sensitivity Of SPE-04 The HP SPE column is based on high quality spherical silica gel and morecomplete bonding process. Below is a comparison using patent blue： As SPE-04 can only make use a portion of the trapped analytes foranalysis， enrichment by SPE column is important for improving detectionsensitivity. By using a 50-mg HP SPE column， a 5-mL sample will end up in1 mL fraction. It is enriched 5 times.