用于分离0.2%杂质的质量导向制备SFC

超临界流体色谱（SFC）是一种快速生长的技术。最初，almostex仅用于热不稳定和手性化合物，现在被认为是一种适用于多种化合物的通用分析和纯化技术。它比常规HPLC和Prep-lc的产量更高，并具有溶剂消耗、耗材和处理成本低得多的绿色优势。SFC与多种检测方法兼容，包括紫外线、电喷雾（ESI）和大气压化学电离（APCI）质谱法。 Mass-Directed Fraction Collection for Preparative SFC Collection of a 0.2% impurity using a Jasco Prep SFC coupled with the expression Compact Mass Spectrometer Mark Hardink *，Frank Riley & Qi Yan， Pfizer； Simon P rosser， Advion；John Burchell & DJ Tognarelli，JASCO Experimental Introduction Supercritical fl u id chromatography (SFC) is a rapidly growing technique. Initially used almost exclusively only for thermal l y labile and chiral compounds， it is now accepted as a versatile an a lytical and purification technique applied across at broad range of compounds. It is higher-throughput than regular HPLC and Prep-LC and offers the green’ advantages of much lower solvent consumption， consumable and disposal costs. SFC is compatible with a wide range of detection 1methods S including UV，electrospray (ESI)and atmospheric pressure chemical ionization (APCI) mass spectrometry. Objective To d e termine the purity of col l ection of a small (0.2%)impur i ty in a concentrated sample matri x using the extracted ion chromatogram (XIC) for mass directed fraction collection. Methods 1. Pre-Purification Analytical： A small aliquot is injected to determine whether the compound target ma s s is present and to measure the UV purity of the sample prior to pur i fication.The combination of t a rget mass being found and the sample 's purity determine whether a sample moves to the preparative stage and which preparative narrow method， based on target retention t i me， will be automat i cally selected for the pur i fication process. 2. Purification： 20 injections of 0.7 mL were made and the target mass extracted using fraction collection based on the method i d e nt i fied in Pre-purification.Mass directed trigge ri ng using XIC for Flavone m/z 223.1. 3. Post-Pur i fication Analytical： A smal l aliquot is injected from each tube of collected fraction material and the final sample purity measured. Instrument Set up JASCO Preparative SFC system with fraction collec t ion and Advion express i on CMS ZDV splittingtees post-UV detection， 1" tee po st VWD spl i ts in the solvent make-up for the fraction collector and travels to 2nd tee that sp lit s flow to the CMS via 100 cm x 0.025 mm PEEKSil. ZDV splitting tee pre-CMS splits in t he LC/MS make-up solvent for ionization and sam pl e e stream from 2nd ZDV tee PEEKSil l i ne. Results Zoom chromatogram of 0.2% Flavone i n 10mg/mL Carbamazepine .MS T r igge r ing w i th XIC Conclusions · The CMS can be simply i nterfaced to both analytical scale and p rep scale SFC using a simple passive split before th e UV detector · Al l fractions co ll ected of each analyte were tested a nalytic a lly and showed that each was 99.9% pure or greater · L i mit determination at 0.2% Flavone in the presence o f Carbamazepine -Using the XIC signal to trigger the fraction collector ， a 0.2 wt % pe a k of Fl a vone was collected a t 100% purity