Application Note Alert

March 2011 Subscribe

Links to technical insights from sponsored Featured Application Notes on Chromatography Online.
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- Janet Kelsey

Featured Application Note:
Determination of BPA in Infant Formula by LC-MS/MS
By Yang Shi, Catherine Lafontaine, Matthew Berube, Francois Espourteille, Thermo Fisher Scientific

A six-minute LC-MS/MS method integrating Thermo Scientific TurboFlow technology is a powerful technique for the direct analysis of Bisphenol A in canned infant formula powder without the need for lengthy sample preparation.

Sample Prep
10-500ppt OCP-OPP Pesticides in Green Tea
John Heim, Mark Libardoni Ph.D, Nobou Ochiai Ph.D and Kikuo Sasamato, LECO

Quantification of PPT level OCP/OPP pesticide residues is described. Analysis by GC-TOFMS presents a fast, accurate, and sensitive method in five types of green tea.

Sample Prep
Highly Sensitive UV Analysis with the Agilent 1290 Infinity LC System for Fast and Reliable Cleaning Validation – Part 1
Edgar Naegele, Katja Kornetzky, Agilent Technologies

This Application Note demonstrates high sensitivity measurement of pharmaceutical compounds with the Agilent 1290 Infinity LC. It also demonstrates a performance comparison of different flow cells with the Agilent 1290 Infinity LC Diode Array Detector (DAD) for highly sensitive UV measurement including calibration, validation, and determination of LOD and LOQ.
Fast Determination of Vanillin and its Synthesis Precursors
Xu Qun, Li Lang, and Jeffrey Rohrer, Dionex Corporation

This note describes a fast HPLC method to determine vanillin and its synthetic precursors for process monitoring and quality control of the two-step synthetic process. The lab also made the separation compatible with MS and used the MSQ to determine the identities of some of the synthesis by products.
Separation of Folic Acid and Related Polar Compounds
Xu Qun, Li Lang, and Jeffrey Rohrer , Dionex Corporation

This note demonstrates an efficient HPLC method for the simultaneous separation and quantification of THP, DNHP, and folic acid on the Dionex Acclaim Mixed-mode WCX-1 column.
Find the Right Balance in UHPLC
Patrik Appelblad, Gora Sharangi, Petra Lewits and Volker Eckert, Merck Millipore

A Purospher® STAR UHPLC column is an excellent and inexpensive tool to achieve fast chromatography and it provides high separation efficiency at moderate back pressure. The stationary phase is well-balanced in its overall chromatographic properties and designed for universal use. Robust methods can easily be developed in a wide pH-range with good column longevity, which gives a low price-per-injection and ultimately cost-efficient assays.
Effectively Separating PEGylated Proteins using BioSep™ Gel Filtration Chromatography Columns
Vita Knudson, Tivadar Farcas, and Michael McGinley, Phenomenex

Efforts were undertaken to evaluate using gel filtration chromatography as a method for purifying PEGylated proteins from their unmodified precursors. Several different proteins and PEGylation chemistries were evaluated on BioSep SEC 2000 HPLC columns. Results show that retention of PEGylated species is directly related to the size of the PEG reagent used; proteins modified with larger PEG moieties generally demonstrate greater resolution from unmodified proteins than small modifications. Such results show the utility of GFC using BioSep 2000 as a means of characterizing and purifying PEGylated proteins.
Quantitation of Perfluorinated Compounds in Human Breast Milk using Selected Reaction Monitoring Assays by LC/MS/MS
Christine Gu, Guifeng Jiang, Robert Szilasie, Stephen Hassan, Allen Zhang, Mark Sanders, Thermo Fisher Scientific

A highly sensitive, accurate and robust SRM-based approach for PFC analysis was developed on a Thermo Scientific PFC-free Accela-TSQ Vantage LC-MS platform. PFCs were accurately and reproducibly detected at ppt levels in neat solution and in human milk.
Improving Mass Load Capacity For Basic Compounds Using Charged Surface Hybrid (CSH) Technology Columns
Kenneth J. Fountain and Hillary B. Hewitson, Waters Corporation

Many modern stationary phases suffer from poor chromatographic performance for basic compounds at low pH, especially when using low-ionic strength mobile phases such as formic acid.
Gelatin characterization by MALS
R.H. Tromp and C. Olieman

Gelatin is the denatured form of collagen, the main component of skin, bone and connective tissues of animals. Its special properties are a sharp sol-gel transition, low sol viscosity and high effectiveness as a protective colloid. This note examines the absolute characterization using multi-angle light scattering.

LC/HPLC

HRMS Qual/Quant: Simultaneous Pharmacokinetic Profiling and Automated Metabolite Identification
Suma Ramagiri, Jeff Miller, Hesham Ghobarah, AB SCIEX

Explore the use of the TripleTOF™5600 System from AB SCIEX for HRMS Quant/Qual workflows in simultaneous in vivo PK and metabolite identification for buspirone following adminstration in rat.


LC/HPLC
One Step Extraction, Cleanup and Direct to Vial Concentration for PCBs in Soil and Sediment
Phil Bassignani, FMS, Inc.

This method determines the concentrations of various PCB congeners and Aroclors in extracts from solid and liquid matrices, including food products. This application provides a unique new option to speed up multiple sample prep processes into one. The FMS PLE (pressurized liquid extraction) system will automatically perform the extraction and sample cleanup using the FMS InCell column, then deliver the extract to the FMS PowerVap for final concentration directly to a vial to be injected directly by the GC system.
PAHs in Seafood by QuEChERS-SBSE-GC/MS
Jeffrey H. Moran, Edward A. Pfannkoch, John R. Stuff, Jacqueline A. Whitecavage, Arkansas Public Health Laboratory and GERSTEL

QuEChERS extraction combined with SBSE-GC/MS provides a highly productive alternative to NOAA Method NMFS-NWFSC-59 2004, currently used for determining PAH levels in seafood. Rather than 14-15 samples per week, the average laboratory would be able to process 40-50 samples per day, while reducing solvent usage and improving detection limits significantly. Limits of quantitation were shown to be < 1ng/g.
Determination of 25-mono-hydroxy-vitamin D2 and D3 in Human Plasma using a Symbiosis™ Pico System: ACN free On-line SPE-LC-MS/MS
Martin Sibum, Spark Holland

To meet the growing demand for determining both 25-mono-hydroxy- Vitamin D2 and Vitamin D3 in one run, a fully automated method has been created, combining on-line SPE and LC-MS in one integrated system (Symbiosis™ Pico). This method requires no manual pretreatment step(s) anymore, just one operator step is required before SPE and LC-MS are executed fully automated in one unattended run. This results in high throughput, low CV’s and high precision.
Improved Recoveries of Polycyclic Aromatic Hydrocarbons (PAHs) as Defined in EPA 550.1 and Simultaneous Removal of Humic Acids from Water Using Strata PAH
Zeshan Aqeel, Seyed Sadjadi, and Erica Pike, Phenomenex

Polycyclic aromatic hydrocarbon compounds (PAHs) are effectively extracted from water samples while humic acids, which often interfere with chromatographic separation, are removed from the sample using a SPE sorbent, Strata® PAH. It was also found that Strata PAH provides consistent, high recoveries of all 16 analytes listed under EPA Method 550.1.

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