Semivolatile calibrations on this column dimension often range from 1.0 to over 100 ng/µL; however, a 0.25 mm ID column usually experiences peak overload as the mass on column approaches 10 ng. As shown in Figure 1, isobars that elute close together-such as benzo[b]fluoranthene and benzo[k]fluoranthene-quickly become unquantifiable as mass on column increases. Under split conditions, the resolution requirement (50% valley) is met for all nine calibration standards, and the peak apices shift less than 0.04 min, indicating only minor peak overload. Conversely, under splitless conditions, the three highest concentration calibration standards fail the resolution criterion. The peak fronting and resulting overlap from column overload make it impossible to generate a linear calibration including these points. Additionally, the peak apex of benzo[b]fluoranthene shifts more than 0.2 min, which could result in an erroneous compound identification.
Initial precision was demonstrated by spiking four 1-L volumes with one Snip and Pour pre-measured standard, each (40 mg). The data for four replicates was collected for 47 mm Disks and 100 mm Disks. The average percent recovery is excellent and meets the criterion specified of 83–101% HEM recovery for both size disks. The standard deviation is better than the criterion specified of 11% for HEM.
BioPharma Compass? is a fully automated solution for the rapid characterization of biopharmaceutical products such as proteins, peptides, RNA, and DNA. This push button solution assists nonspecialist operators to generate high quality, accurate data for automatic comparison with laboratory reference standards. Automated, visual reports are then generated for each sample and important information regarding a products purity and identity can be observed at a glance. In this application note, we will apply the BioPharma Compass workflow to the QC characterization of two proteins including intact IgG1 and digested transferrin.
The standards are commercially available from Wellington Laboratories Inc. (Ontario, Canada): TF-TCDD-MXB.
Deans switch two dimensional gas chromatography is a powerful tool for identification and quantitation of trace components in a complex matrix. With this setup, operators no longer work in the dark. MDGCsolution software makes the heart-cut easy and straightforward.
Shiseido succeeded in development of CAPCELL CORE ADME S2.7, a novel stationary phase with an adamantyl group having a cage structure. This is characterized as alkyl group; therefore, the packed column is still easy to use just as a reversed-phase column.
Hydrophilic interaction chromatography (HILIC) was introduced more than two decades ago and has garnered much attention. Characterized by a hydrophilic stationary phase used in combination with an aqueous organic mobile phase, numerous improvements have been achieved and HILIC is now considered as an attractive alternative to reversed-phase phase liquid chromatography (LC) for many applications. HILIC provides several advantages over reversed-phase LC for the analysis of polar compounds, including higher retention of polar metabolites, enhanced mass spectrometric sensitivity, moderate back-pressure - even at high flow rates, or when used with sub-2-µm particle size - and orthogonal selectivity. Several important technical developments have been proposed during the last decade that foster its use in metabolomics. This review presents an overview of the most recent technical improvements and applications of HILIC analysis in untargeted clinical metabolomics and discusses important practical considerations, including the selection of the optimal column chemistry, appropriate eluents, sample preparation, and data analysis.
Shimadzu Europa GmbH
A chronological examination of GC is presented here, with a look at where the technique is heading and how it can be used to advance environmental sustainability.
Here is a step-by-step approach to investigate the source of ghost peaks in a gradient LC method.
A sensitive and selective liquid chromatography spectrometry mass spectrometry (LC–MS–MS) method to determine clenbuterol-like beta agonist residues in human hair was developed and validated.
The past decade has brought exponential growth in the number of mass spectrometry (MS) ionization techniques based on desorption and ionization (DI) processes. Here, the three key applications for DI are discussed: rapid, in situ screening; direct analysis of extracted samples or of planar chromatography spots; and scanning samples along x and y axes.
This fit-for-purpose LC–MS based method provides fast analysis of four mycotoxins using standard HPLC equipment with a pentafluorophenyl SPP column.
When selecting the optimum phase for SEC separations, several key column parameters must be considered carefully.
An investigation of C18 and phenyl-hexyl column chemistries for definitive identification of 13 synthetic cannabinoid metabolites in patient samples.
When selecting the optimum phase for SEC separations, several key column parameters must be considered carefully.
An investigation of C18 and phenyl-hexyl column chemistries for definitive identification of 13 synthetic cannabinoid metabolites in patient samples.
Recent advances in chiral stationary phases have enabled higher efficiency and faster separations in studies of the differing enantiomeric activity of pesticides, their environmental transformation, and the degradation of pollutants in general.
As clinical diagnostic assays move to LC–MS–MS, the emphasis has turned to emerging stationary phases that use alternative mechanisms of retention to separate the analyte–interference critical pairs.
As clinical diagnostic assays move to LC–MS–MS, the emphasis has turned to emerging stationary phases that use alternative mechanisms of retention to separate the analyte–interference critical pairs.
This article provides useful tips for smooth validation of multi-analyte LC–MS-MS methods and summarizes important validation outcomes for 295 analytes, including more than 200 mycotoxins.
In this article, two sample handling and sample preparation methods for saliva samples are presented and discussed. Both methods were applied for determining the presence of lidocaine in saliva.
A focus on untargeted UHPLC–MS/MS lipidomics with data independent acquisition using SWATH technology. This article explores the wide-ranging potential and peculiarities of SWATH–MS hyphenated with UHPLC for the profiling of lipidomes of various biological samples.
Therapeutic peptides represent one of the fastest growing segments in the pharmaceutical market. To bring these products to the market in a consistent manner, high quality is a major concern and requires stringent quality control (QC) methods. This article discusses the potential of zwitterionic chiral ion-exchangers to support peptide analysis and quality control as a flexible complementary tool to monitor the stereochemical integrity and chemical modifications.
Therapeutic peptides represent one of the fastest growing segments in the pharmaceutical market. To bring these products to the market in a consistent manner, high quality is a major concern and requires stringent quality control (QC) methods. This article discusses the potential of zwitterionic chiral ion-exchangers to support peptide analysis and quality control as a flexible complementary tool to monitor the stereochemical integrity and chemical modifications.
Therapeutic peptides represent one of the fastest growing segments in the pharmaceutical market. To bring these products to the market in a consistent manner, high quality is a major concern and requires stringent quality control (QC) methods. This article discusses the potential of zwitterionic chiral ion-exchangers to support peptide analysis and quality control as a flexible complementary tool to monitor the stereochemical integrity and chemical modifications.
Therapeutic peptides represent one of the fastest growing segments in the pharmaceutical market. To bring these products to the market in a consistent manner, high quality is a major concern and requires stringent quality control (QC) methods. This article discusses the potential of zwitterionic chiral ion-exchangers to support peptide analysis and quality control as a flexible complementary tool to monitor the stereochemical integrity and chemical modifications.
Therapeutic peptides represent one of the fastest growing segments in the pharmaceutical market. To bring these products to the market in a consistent manner, high quality is a major concern and requires stringent quality control (QC) methods. This article discusses the potential of zwitterionic chiral ion-exchangers to support peptide analysis and quality control as a flexible complementary tool to monitor the stereochemical integrity and chemical modifications.