title: Implementation of high-temperature superficially porous technologies for rapid LC-MS/MS diastereomer bioanalysis.
abstract: BACKGROUND
  The fast-paced nature of the pharmaceutical industry requires robust bioanalytical methods to endure the high-throughput sample demands of the production environment.
  
  
  RESULTS
  A rapid, accurate and precise LC-MS/MS method was developed for the quantitation of a diastereomer quartet in human plasma. Virtually all of the phosphatidylcholine and most of the lysophosphatidylcholine from human plasma were removed using a phospholipid-removing protein precipitation 96-well plate. An Agilent Poroshell SB-C18 2.1 × 50 mm superficially porous column was used at 100°C and 1.2 ml/min to separate a diastereomer quartet in <2.5 min. Peak shape, retention and resolution were maintained over nearly 200 extracted bioanalytical samples under these separation conditions. The method was tested for accuracy and precision; the assay inter-run accuracy and precision were minus 7.2-0.7% and 2.1-11.9%, respectively (n = 18).
  
  
  CONCLUSIONS
  The application of the superficially porous column resulted in twofold response increase and a 2.6-fold reduction in cycle time compared with a 3.5-µm column performing under comparable resolution conditions.
authors: Merck Research Labs, Summit, NJ 07901, USA. jennifer.cunliffe@merck.com
authors: Jennifer M
authors: JM
authors: Cunliffe
authors: Jim X
authors: JX
authors: Shen
authors: Xianrong
authors: X
authors: Wei
authors: Daniel P
authors: DP
authors: Dreyer
authors: Roger N
authors: RN
authors: Hayes
authors: Robert P
authors: RP
authors: Clement
mesh_terms: D001774:Blood Chemical Analysis / Q000295:instrumentation* / Q000379:methods; D002851:Chromatography, High Pressure Liquid / Q000295:instrumentation* / Q000379:methods; D003521:Cyclopropanes; D004151:Dipeptides / Q000097:blood*; D006801:Humans; D007930:Leucine / Q000031:analogs & derivatives; D008244:Lysophosphatidylcholines / Q000097:blood; D010713:Phosphatidylcholines / Q000097:blood; D011392:Proline / Q000031:analogs & derivatives; D013237:Stereoisomerism; D013450:Sulfones / Q000097:blood*; D053719:Tandem Mass Spectrometry / Q000295:instrumentation* / Q000379:methods; D013678:Technology, Pharmaceutical / Q000295:instrumentation* / Q000379:methods; D013696:Temperature; D014508:Urea
chemical_list: D003521:Cyclopropanes; D004151:Dipeptides; D008244:Lysophosphatidylcholines; D010713:Phosphatidylcholines; D013450:Sulfones; C552043:narlaprevir; D014508:Urea; D011392:Proline; D007930:Leucine