DiscovIR-LC™

Reversed Phase LC-IR Spectra Collected in 

Real Time With Physical Solvent Removal

 

Fifty microliters of a 0.5 mg/mL solution of a four component mixture were injected onto a C18 Nova-Pak 75 mm x3.9 mm I.D. column. A 10 minute gradient from 98%H2O/CH3OH to 100% CH3OH at a flow rate of 1 mL/minute was employed. 

New DiscovIR-LCTM system from Spectra Analysis is able toafford total solvent

removal from a reversed-phase gradient run (2% to 100% organic) with 

no changein the operational set points of the system. Solid phase Transmission 

FTIR Spectra are acquired continuously throughout the run. 

 

 

 

 

Figures 1-2 show the chromatogram and FTIR spectra of the eluants 

 

 

How Does It Work?

Upon exiting the LC column, solvent is removed and theeluants are deposited onto a sample collection disk. Theinfrared ZnSe disk rotates under the deposition tip toresult in a spiral track of deposited samples. A beam ofinfrared light from an interferometer passes throughthe disk along the deposition track, and infrared spectral information are acquired by a MCT detector.

 

 

Key Applications :

•  Deformulation

•  Co-polymer Compositional Drift

•  Extractables & Leachables

•  Minor Component Identification

•  Chemical Troubleshooting

•  Degradation / Failure Analysis 

 

 

Key Benefits : 

A Breakthrough Detector Technology

DiscovIR-LC is a “breakthrough” (solvent removing) FTIR detector technology, providing solid-phase analysis of HPLC (HighPerformance Liquid Chromatography) and SEC (Size ExclusionChromatography) separations. DiscovIR-LC represents the first fully-automated high performance HPLC-FTIR detection system capable of achieving the kind of rigorous, repeatable qualitative analyses that pharmaceutical, polymer chemists and other industry customers require. By providing an on-line chemistry solution, DiscovIR-LC increases the productivity of a company’s most valuable processes: product development, process control and troubleshooting,quality control (incoming and outgoing), patent protection and competitive analysis.

 

Micro-Deposition Improves Analysis

DiscovIR’s unique temperature controlled and vacuum deposition method ensures that results are accurate and reproducible. Eluted peaks are first deposited in a film onto a rotating IR-transparent disc. Next, an infrared beam passes through each concentrated spot and the detector automatically collects spectra data.

 

Concentrates Analytes in Minimal Area

Cryogenic temperature control of the Sample Disc minimizes the area of the deposited analyte. This results in a thicker sample layer and therefore higher sensitivity of the absorbance spectrum.

 

Retains Entire Chromatographic Run

The entire chromatographic run is applied as a solid deposit onthe Sample Disc, preserving the resolution of the separation. Therefore, the entire run is available to be scanned again in order to investigate subtle features and improve signal-to-noise. The speed of the rotating Sample Disc can be adjusted to match concentration of the deposited sample. 

System Overview
Operating Principle	Direct deposition of column eluent on moving ZnSe sample disc
IR Spectrometer	Built-in FTIR
IR Detector	0.1 mm MCT
Wavenumber Range	4000–650 cm-1
Data Collection	Real-time, with post-run analysis available
Spectrum Type	Transmittance through disc and solid-phase sample
Window Capacity	12-24 hours of chromatography
Window Temperature	-100°C to +50°C
Data Station
Platform	Windows™ XP
Spectroscopy Package	Grams32
Standard Features	• Real-time and post-run data collect
	• Chromatographic / spectral workup
	• Band chromatograms for chemical classes
	• Ratio chromatograms for profiling trends
Library Search	Library Search Software included
	Spectra compatible with all solid phase FTIR Libraries
DiscovIR-LC Configuration
Sample Delivery	Multi-Step Desolvation Interface
Flow Rates Accepted	0.25 to 1.5 mL/min
Compatible Solvents	Water, ACN, Methanol, THF, Chloroform
Compatible Additives	Volatile buffers (ammonium carbonates, acetates, formates), trifluoroacetic acid (TFA), triethylamine (TEA)
Sensitivity	Typically 1ug per component
Chromatograph	Any Liquid Chromatograph System (supplied by user)

 

Immobilizes Entire Run 

Since the entire chromatographic run is applied to the Sample Disc, the resolution of the separation is not lost as in some collection systems. Additionally, the entire run is available to be scanned again to investigate subtle features or improve signal-to-noise. The speed of the rotating Sample Disc can be adjusted to match concentration of the deposited sample.

Applications

 Copolymer Characterization

 •  Variability of Polymeric Excipients and Its Effect on Drug Delivery Performance

 •  LC-IR Characterization of Polyolefins

 •  Polymer Additives Analysis

 •  Copolymer Compositional Drift Measurement

 •  Characterization of a Hot-Melt Adhesive by LC-IR

 •  Oxidative Degradation of Polyethyleneglycol (PEG) studied by LC-IR

 •  Deformulating UV Coating System by LC-IR Technology

 Characterizing Pharmaceutical Excipients

 •  Variability Of Polymeric Excipients And Its Effect On Drug Delivery Performance

 •  Analysis of Polymeric Excipients in Pharmaceutical Formulations

 •  Oxidative Degradation of Polyethyleneglycol (PEG) studied by LC-IR

 •  Characterization of Polymer Excipients by SEC-IR

 

 General Analytical Needs

 •  Lubricants Analysis

 •  IR Applied to Isomer Analysis

 •  Determining Benzene Ring Substitution Patterns from IR Spectra

 •  Getting Quality LC-IR Spectra from 1% Mixture Components

 •  Reversed phase LC-IR collected in real time

 •  Selective Detection using Band Chromatograms