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ePaper created 2015-07-06, 08:54:49 | version 1.39.0
MassSpectrometry LABBOOK 2015 21 HYBRID/MASSSPECTROMETRY LABBOOK 2015 With the new UF Qarray, Shimadzu has achieved a technologi- cal breakthrough that combines high, apparently contradictory, demands such as increased sensitivity and robustness of LCMS systems. New applications become conceivable and feasible when the world's best sensitivity is combined with high-speed parameters in the LCMS-8060. The smallest sample amounts in complex matrices ± or any low sample concentrations that need to be further diluted to decrease matrix effects ± are now detectable. As an example, (d6-)-no- repinephrine is discussed here, of which just 5 ppt can be extracted from plasma and still be detected (Figure 4). Uniform software for all triple-quadrupole models The increasing demands for quantification at trace levels in clinical research, food analysis and in other market segments, place high demands on instrument technology as well as on users. The LCMS-8060 offers not only technological advancements at the highest level, but also continuous adaption of the instrument software to changing user needs. The LCMS-8060, as well as all other triple-quadrupole models and Shimadzu's HPLC/UHPLC systems, is controlled using the LabSolutions LCMS-software. A uniform user interface enables overview and control of the hardware as well as simultaneous processing of initial analysis results. Additional functions The excellent speed parameters of the LCMS systems and the advanced software enable the implementation of helpful additional functions such as the so-called Synchronized Survey Scan (SSS). This additional MS/MS experiment is triggered when a predefined intensity in the associated experiment is exceeded. As an example, it is pos- sible with this function to carry out an MRM and the corresponding qualitative production scan almost simultaneously within one analysis run, without compromising the accuracy of the quantitative analysis. For example, extracted whole blood samples spiked with flunitraze- pam (Figure 5) demonstrate impressively that, despite the simul- taneously measured SSS, the peak reproducibility attained is very good. This is only possible with the help of high UF scan speeds that assure generation of a sufficient number of data points, necessary to describe the peak accurately. In addition to the quantitative results, high-quality mass spectra are obtained that correlate well with library spectra, even at low concentration. This enables une- quivocal peak characterization. Workload reduction due to fully automated MRM optimization The improved, fully automated MRM optimization enables a real reduction in workload. While it was still necessary with earlier versi- ons to determine and enter the parent ion manually, it is now suffi- cient to indicate the molecular weight. The software then calculates the protonated or deprotonated ions as well as all possible adducts and takes these into consideration during optimization. With the LCMS-8060, Shimadzu has further advanced the MS technologies of its predecessor models. Particular attention has been paid to robustness and straightforward operation. Outstan- ding performance of the instrument is thus guaranteed over a long period of time. Figure 2 The Qarray is the key to higher sensitivity. Figure 4 5 ppt norepinephrine-d6 in plasma, calibration curve 5 ± 2000 ppt. Figure 5 Flunitrazepam in whole blood. Figure 3 Comparison of the signal-to-noise ratio of omeprazole. LABBOOK 201521 Figure 45 ppt norepinephrine-d6 in plasma, calibration curve 5 ± 2000 ppt.