Round-robin evaluation of a solid-phase microextraction–gas chromatographic method for reliable determination of trace level ethylene oxide in sterilized medical devices

2008 ◽  
Vol 22 (2) ◽  
pp. 136-148 ◽  
Author(s):  
Thomas Harper ◽  
Lisa Cushinotto ◽  
Nancy Blaszko ◽  
Julie Arinaga ◽  
Frank Davis ◽  
...  
Keyword(s):  
Ethylene Oxide ◽  
Medical Devices ◽  
Solid Phase Microextraction ◽  
Chromatographic Method ◽  
Solid Phase ◽  
Round Robin ◽  
Trace Level ◽  
Reliable Determination ◽  
Gas Chromatographic Method

scholarly journals Determination of Low-Level Residual Ethylene Oxide by Using Solid-Phase Microextraction and Gas Chromatography

2002 ◽  
Vol 85 (6) ◽  
pp. 1205-1209 ◽  
Author(s):  
Kamal Ayoub ◽  
Leonard Harris ◽  
Bill Thompson
Keyword(s):  
Gas Chromatography ◽  
Ethylene Oxide ◽  
Medical Devices ◽  
Solid Phase Microextraction ◽  
Capillary Column ◽  
Solid Phase ◽  
Extraction Temperature ◽  
Absorption Time ◽  
Low Level

Abstract Current methods of analysis for ethylene oxide (EO) in medical devices include headspace and simulated-use extractions followed by gas chromatography with either a packed or a capillary column. The quantitation limits are about 0.5–1.0 μg/g for a packed column and about 0.1–0.2 μg/g for a capillary column. The current allowable levels of EO on medical devices sterilized with EO gas as outlined in International Organization for Standardization (ISO) 10993-7 may be significantly reduced from current levels by applying the ISO Draft International Standard 10993-17 method for establishing allowable limits. This may require EO test methods with detection and quantitation limits that are much lower than those of the currently available methods. This paper describes a new method that was developed for the determination of low-level EO by solid-phase microextraction using the direct-immersion method. Factors such as temperature and stirring were found to affect absorption efficiency and absorption time. A low extraction temperature (about 6°C) was found to be more efficient than room-temperature extraction. Stirring was found to reduce absorption time by about 50%. Under these conditions, detection and quantitation limits of 0.002 and 0.009 μg/g, respectively, were obtained by using a capillary column. As a result, this method makes compliance with lower EO limits feasible.

Improved determination of phenobarbital, primidone, and phenytoin by use of a preparative instrument for extraction, followed by gas chromatography.

1979 ◽  
Vol 25 (8) ◽  
pp. 1373-1376 ◽  
Author(s):  
L M St Onge ◽  
E Dolar ◽  
M A Anglim ◽  
C J Least
Keyword(s):  
Chromatographic Analysis ◽  
Chromatographic Method ◽  
Solid Phase ◽  
Correlation Coefficients ◽  
Specific Method ◽  
Sensitive Detector ◽  
Gas Chromatograph ◽  
Solid Phase Extraction Cartridge ◽  
Gas Chromatographic Method

Abstract A microprocessor-controlled automatic extractor, (PREMTM I) is described with which lipophilic components may be extracted from physiological fluids by means of a selective, solid-phase extraction cartridge, and the extracts presented in dry form for subsequent analysis. This instrument has been successfully evaluated for the extraction of phenobarbital, primidone, and phenytoin from human serum before chromatographic analysis. We describe a specific method for determination of these anticonvulsants, involving the PREP I and analysis, after flash-heater methylation, in a gas chromatograph equipped with a nitrogen-sensitive detector. Absolute recoveries ranged from 90 to 102%. Within-day and day-to-day precision (CV) ranged from 4 to 7% for all three drugs in therapeutic concentrations. Comparison of this method with results obtained with a liquid--liquid micro-scale extraction and a similar gas-chromatographic method resulted in correlation coefficients of 0.988 (phenobarbital), 0.978 (primidone), and 0.982 (phenytoin). These drugs in therapeutic concentrations can be simultaneously extracted and measured with confidence.

Determination of Residual Ethylene Oxide in Spectinomycin Hydrochloride Bulk Drug by Dynamic Headspace Gas Chromatography

1993 ◽  
Vol 76 (2) ◽  
pp. 313-319
Author(s):  
Tore Ramstad ◽  
Lisa S Miller ◽  
Virginia N Thomas
Keyword(s):  
Detection Limit ◽  
Ethylene Oxide ◽  
Chromatographic Method ◽  
Headspace Gas Chromatography ◽  
Dynamic Headspace ◽  
Relative Standard ◽  
Headspace Gas ◽  
Bulk Drug ◽  
Gas Chromatographic Method

Abstract A dynamic headspace gas chromatographic method was developed for the determination of residual ethylene oxide (EtO) in a pharmaceutical bulk drug, spectinomycin hydrochloride. The recommended column is PoraPLOT Q; PoraPLOT U was demonstrated to be equivalent. A detection limit of 2 ppb was achieved, and linearity was established to the highest value tested (5 ppm). The detection limit was 2-3 orders of magnitude lower than that achieved in previously published methods for EtO in pharmaceutical bulk drugs. Precision studies yielded relative standard deviations ranging from 2 to 10% over the 10-575 ppb concentration range. The method was applied to support EtO sterilization studies conducted at The Upjohn Company and was implemented for routine use. The sterilization studies demonstrated that residual levels of EtO <10 ppb are achievable.

Determination of trace phenolic acids in fruit juice samples using multiple monolithic fiber solid-phase microextraction coupled with high-performance liquid chromatography

2016 ◽  
Vol 8 (18) ◽  
pp. 3831-3838 ◽  
Author(s):  
Miao Pei ◽  
Xiaojia Huang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Phenolic Acids ◽  
Solid Phase Microextraction ◽  
High Performance ◽  
Analytical Approach ◽  
Fruit Juice ◽  
Solid Phase ◽  
Trace Level

A simple and sensitive analytical approach of MMF/SPME-LD-HPLC/DAD was proposed for the determination of trace level of phenolic acids in fruit juice samples.

scholarly journals Variables Affecting Simulated Use Determination of Residual Ethylene Oxide in Medical Devices

2001 ◽  
Vol 84 (2) ◽  
pp. 512-518 ◽  
Author(s):  
Duane T Centola ◽  
Kamal I Ayoub ◽  
Nelson T Lao ◽  
Hollington T C Lu ◽  
Barry F J Page
Keyword(s):  
Ethylene Oxide ◽  
Medical Devices ◽  
Working Group ◽  
Round Robin ◽  
Contributing Factors ◽  
Initial Water ◽  
Short Sample ◽  
Sample Extraction ◽  
Relevant Variables

Abstract In autumn 1993, AAMI/ST/WG 63, Sterilization Residuals Working Group undertook the task of studying factors involved in determining the amount of residual ethylene oxide in medical devices after sterilization and developing a protocol for controlling the relevant variables. The protocol was evaluated by conducting a round robin study consisting of 8 participating laboratories from around the country. Results of this round robin study demonstrated the range over which results may vary despite controls placed on the time and temperature at which determinations were conducted. The data from the study suggest that small, random variations in technique during short sample extraction times can lead to variability in the results. Variables such as initial water temperature, oven temperature, weighing of sample, and length of extraction should be carefully controlled. Inherent variations in the material composition of similar devices are possible contributing factors. The efforts of this working group and the subsequent evaluation and discussion of its findings are presented.

Sign in / Sign up

Export Citation Format

Share Document