Table of Contents

WINTER QUARTERLY MEETING

Title: Trials and Tribulations of PCB Analyses

Watch your mail for a  flyer with the speaker bio and directions or visit the MCF website at www.minnchrom.org

ABSTRACT

Polychlorinated biphenyls (PCBs), manufactured in the United States between 1930 and 1977, are ubiquitous environmental pollutants. The Toxic Substances Control Act (TSCA), specifically singles out PCBs, and mandates U.S. EPA to regulate their manufacture, processing, distribution in commerce and logically their disposal or destruction. PCBs consist of 209 distinct chlorine substituted biphenyl molecules (congeners) of which two thirds appear at significant concentration levels in different commercial mixtures or products (most often manufactured in the U.S. by Monsanto and marketed under the trade name Aroclors). PCB contamination of environmental media (soil, water, air) and organisms arose from spills resulting from closed system electrical capacitors and transformers, hydraulic fluids, etc. and from open-end uses in materials such as carbonless paper, plastics, landfills, lubricants, etc.

This talk will focus on PCB analytical procedures (many interesting and unique to PCBs) specifically sample collection, extraction, extract clean-up, analysis, data reduction and QA to provide a PCB result - total PCBs, specific selected congeners, commercial mixtures (Aroclors), etc.

Two selected references provide insight in PCB measurements:

1. Erickson, Mitchell D., "Analytical Chemistry of PCBS", 2nd edition, CRC/Lewis Publishers, 1997.

2. Frame, George, "Congener-Specific PCB Analysis", Anal.Chem.(news and Features 69, 468A (1997).

FROM THE PRESIDENT'S DESK

WardSwanson

As a person in the quality assurance business, I am constantly reviewing processes and procedures and looking for ways to upgrade and improve the status quo. Occasionally, I will even shine that light upon non-occupational areas such as the MCF.

Last year, in an effort to upgrade quality and stay current with the competition, the board voted to increase the dollar amount of our undergraduate research award. The results have been positive, as we saw fairly significant increase in the number of qualified applicants.

In a similar vein this year, the board has agreed to make a slight increase in the honorarium we award to each speaker we invite to our quarterly meetings. This decision was made based on input from several sources indicating we had fallen slightly behind the "industry average". Now as an elected official I must answer the question: "How do you plan on paying for this?"

Read my lips: There will be no new fee increases!

Increased education and Symposium attendance along with improved vendor and advertising support have made the upgrades possible, with minimal pain.

I believe these improvements will help in keeping our organization at the top of its game as we move into the future. I look forward to seeing at the next quarterly meeting.

MUSINGS ON THE 40th EASTERN ANALYTICAL SYMPOSIUM

Brian Leafblad

Earlier this month, I had the opportunity to attend the Eastern Analytical Symposium in Atlantic City on October 1-4. Overall, I would rate my first experience at EAS very high. Despite a certain amount of uneasiness for everyone that was flying to the east coast so soon after September 11, the conference was well attended and seemed to go off without a hitch. EAS was smaller than other national conferences such as PITTCON or ACS national meetings that I have attended, but the quality seemed higher. There was a good mix of topics from the standard meeting fare of spectroscopy and chromatography to forensic science of a homicide case and the conservation of cultural art.

One interesting topic was a Countercurrent Chromatography symposium chaired by Ian Sutherland of Brunel University in the UK. This technique uses a column (open tubular) with typical dimensions of 1mm I.D. x 50 m. The column is wrapped around a rotating drum which also rotates around a second point, for a "planetary orbit" type of movement. The column is filled with a nonpolar solvent, for example, and the sample is dissolved in a polar solvent. After the sample is injected, the nonpolar solvent is pumped through the column as in a typical HPLC analysis. The difference between this technique and HPLC is that here there is a plug of liquid in the column that is immiscible with the solvent used as the mobile phase. When an instrument is turned on, the rotation of the column spreads out the solvent of the original injection plug against the part of the column furthest from the rotation point. The result is a liquid-liquid extraction throughout the length of the column, with the movement of the analyte controlled by the partitioning between the two liquids. As such, there is no stationary phase to equilibrate or clean, and the column can be reused indefinitely. The main benefit of this technique is the column capacity, as it is routinely used in France for drug purification. The main drawback is time. A typical run can easily take 12 hours.

I also attended a class titled Analytical Data Analysis by Statistical Methods, taught by Dr. Zenaida Otero-Gephardt of Rowan College in Glassboro, NJ. If you haven't ever taken a statistics course, or like me you have forgotten most of what you learned in college statistics, I would highly recommend you take one designed for the analysis of lab data. We do simple things like averages, standard deviations, linear range determination, etc. all the time. But, we also have standard procedures such as running a sample in triplicate, or doing five replicate analyses on each of two days for validation purposes. Why do we do it that way? Is repeating an analysis really going to improve the quality of the data? And if so, how many times do we have to repeat it to get acceptable errors? Or, you may need to determine the effect of three different variables on a data set. How do you design your experiments to determine if two of the variables are inter-related? Being able to statistically evaluate your data will help you answer these type of questions. No groaning, I know math in general is boring for a lot of people and statistics in worse. But understanding the how and why of what you are doing can save you a lot of time and frustration, while increasing the quality of your work.

AAPS MEETING

Ravi Ravichandran

In times of serious travel restrictions imposed by corporations due to slow economy, I should say that I was one of the few fortunate ones who got to travel to Denver to attend the American Association of Pharmaceutical Scientists ( AAPS) in Denver during October 21-25. This was my first AAPS meeting. I am given to understand that the attendance at the AAPS meetings is about 10,000 conferees - nowhere near Pittcon, but still quite respectable. This year I heard that the attendance dropped to about 50%! The Exposition had many empty booths. I guess it was due to the slow economy and the inherent apprehension after September 11.

The plenary session on Monday was quite similar to the Keynote address we are used to in MCF Spring Symposium. No other concurrent sessions were scheduled during the plenary session. Of course the speakers focused on what is ahead of the Pharmaceuticals Industry as the new century unfolds.

T'here were nearly 1000 posters - of course I did not have time to closely scrutinize all the posters. About 100-150 of them were in the Chromatography category. The posters were mainly from academia and small pharmaceutical research companies. Large companies had minimal representation in the posters as far as I could see.

I did not see any new instrumentation except a Circular Dichroism(CD) detector made by Jasco. This can serve both as a UV detector and Circular Dichroism(CD) detector. The manufacturer claims that the detector will enable one to determine the enantiomeric purity without doing any chiral separation. This may not be new to those who went to Pittcon this year.

The biggest talk on the exhibit floor was 21CFR Part 11 compliance. For those of you who are not familiar with the jargon - this is the Code of Federal Regulations that deals with electronic data and signatures. FDA regulated industries, pharmaceuticals, nutraceuticals and medical devices are expected to make sure that their electronic data acquisition and storage practices comply with this regulation. Incidentally, I read in a publication that EPA is considering using similar regulations with regard to electronic data. One more thing for the chemists at the bench and QA folks to worry about!

The registration fee was rather stiff - about $600 for nonmembers. MCF Spring Symposium is a bargain every which way you look at - for the $75 registration fees, the attendees get a year of membership, a lot of food and a handsome gift. There was nothing like that to speak of at the AAPS meeting. The 2002 AAPS meeting will be held in Toronto, Canada.

Beginning Gas Chromatography
January 8-10, 2002...

Registration Deadline Dec 28, 2001.

Use of Designed Experiments (DOE)
 in Chromatographic Applications
February 5-7, 2001...

Registration Deadline Jan 24, 2002.