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Chromatography Quiz No. 6

Chromatography Quiz #5 Results
We would like to congratulate the grand prize winner of our last newsletter’s Carbamate Chromatography Quiz: June Black from the Pennsylvania Department of Environmental Protection! 
She has won, and will shortly be receiving, an extensive California Wines Gift Basket!  Additionally, for this quiz all of our participants will each be receiving a $25 gift card from Bevmo! Again, we would like to thank you all for your submissions.  
The correct answer for the modified Carbamate chromatogram: The system was improperly equilibrated at a higher percentage of methanol (50:50 Water:Methanol) prior to injection.  After injection, the gradient program began with normal starting conditions (85:15 Water:Methanol). For the less retained compounds, the improper conditions on the column at the time of injection will push them through faster, causing coelutions.  Longer retained compounds are less affected by starting conditions of the column, and impacted more by the gradient (which was correct) so you see less of an effect on the later part of the chromatogram. 
Thank you! 
Pickering Labs
Chromatography Quiz #6:
Identify the error made when running the Aflatoxins chromatogram below and win a prize!  Simply email your answer as well as your full contact information to Rebecca at rlsmith@pickeringlabs.com by March 31st in order to win.  You will receive email confirmation that your submission has been received.  The troubleshooting answer and winner congratulations will be published in the next issue (to be anonymous, please notify Rebecca in submission). 

Aflatoxins Analysis by AOAC Official Method 2005.08
LCTech Standard: 0.25 ng B2, G2 and 1.0 ng B1, G1 injected on-column in both chromatograms
LCTech Analytical Column: 150 x 4.6 mm; RP C18 (P/N 10522)
LCTech Guard Column: 8 x 4 mm (P/N 10523; holder P/N 10750)
Normal Operating Conditions: (for reference only, condition changes may be reflected in chromatogram)
Column Temperature: 36 °C
Mobile Phase: Water/methanol/acetonitrile 55/30/15
Isocratic Flow rate: 1.3 mL/min
Post-column conditions:
Photochemical Derivatization: 254nm UV low pressure lamp (LCTech UVE derivatizer, Pickering P/N 1100-3347)
Detection: Fluorometer:  ex 365 nm, em 460 nm

Pinnacle Preventative Maintenance

Keep your Pinnacle in good condition and minimize downtime by performing annual maintenance. Performing Preventative Maintenance on your Pinnacle PCX is easy to accomplish with the Kits and Instruction we provide. Refer to the Maintenance Section of the Pinnacle Manual for details on performing the maintenance. Contact Pickering Laboratories Technical Support with any questions. 800-654-3330, 650-694-6700, or email support@pickeringlabs.com
Below you can find a general maintenance schedule. Your maintenance schedule will depend on usage. If you use the Pinnacle PCX 24×7, you may want to perform the Preventative Maintenance more often.

Maintenance Schedule

Routine Maintenance

         Check for leaks every day
         Replace Flush and Piston Wash reservoirs every week
         Record operating pressures in a daily log book

Preventative Maintenance

         Replace Valve and Pump Seals every 12 months
         Replace the 10um Reagent Frits every 3 months
         Change the tubing every 24 months

Part Numbers

1000-1003               Kit, PM Service, Pinnacle Single Pump (Pump seals, Valve seals, and replacement filter)
1000-1004               Kit, PM Service, Pinnacle Dual Pump (Pump seals, Valve seals, and replacement filter)
1100-0500               Tubing Kit, Pinnacle Dual Pump
1100-0501               Tubing Kit, Pinnacle Single Pump
1452-0122               Pump Seal Kit, Pinnacle
1452-0200               Valve Seal Tool, Pinnacle (Tool only)
1452-0201               Valve Seals kit, Pinnacle (Seals only)
1452-0202               Valve Maintenance Kit, Pinnacle (seals and tool)
3102-9040               Replacement Reagent 10um Filter
1452-0200               Valve Seal Tool

Parts Lookup

Please try our Parts Lookup on our website if you ever need to find a part number. The Parts Lookup is located on our website. Start at http://www.pickeringlabs.com/
Select Parts Lookup under the Service & Support menu
Or, you can also find the Parts Lookup under the Products menu.
Select the Parts Lookup from the Replacement Components menu on the left side of the page.
Next, choose which instrument you are using.
Once you are in the Parts Lookup, simply click on a part or drag you mouse over the part of interest to see the part numbers.

Sincerely,
David Mazawa
 
Technical Support Chemist
Pickering Laboratories, Inc.
1280 Space Park Way
Mountain View, California 94043 USA
Phone: 650-694-6700, ext. 710
Fax: 650-968-0749

Herbal Remedy

By Michael Pickering
Echinacea purpurea, often called a coneflower, has long been used to ameliorate the symptoms of upper respiratory problems caused by viruses and allergies.  The most common form available in the San Francisco Bay Area is in a tablet called Airborne®.  My wife and daughters always have it on hand.  However, if I ingest a tablet, it worsens my symptoms.  I reasoned that the effect was due to the residual incorporated plant material aggravating my hay fever.  So I decided to test the theory by making a tincture wherein the plant material could be categorically removed. 
When water is the extraction solvent, the product is called an infusion and is taken as a hot “tea.”  My solvent of choice for herbaceous tinctures is potable ethanol (190 proof), although as low as 60 proof may be used.  The Everclear® available in California is only 150 proof.  The same brand in Oregon and Nevada is 190 proof, so I had my Oregonian daughter get me some.  That allowed me to filter out the plant residue.  The experiment provided a useable form of Echinacea that is free of allergic side-effects.  My recommended dose is one teaspoon.  I share the extract with my coworkers, friends, and relatives, who all acclaim its efficacy.  One friend actually claims to be allergy-symptom free.
The flower is an annual which my wife and I cultivate in our garden.  Our two plants provide enough cones per season to make 2 liters of solution.  At Pickering Labs, we recently purchased some Echinacea from an herbal supply vendor as a sample for a multi-mycotoxin study, and rather than cones it was supplied as the plant root, called Black Sampson Root. 
Herbal Tincture Preparation:
          Put 100 g dried herbs into a sufficiently sized jar.
          Add 500 mL of 190 proof alcohol.
          Seal, and place on shaker for three days.
o       Note: Longer contact time is recommended for lower proof alcohol.  Two weeks is recommended for 60 proof, for example.
          Filter using a 0.45 μm filter.

Echinacea purpurea

Silk Stockings

By Michael Pickering
Silk stockings were originally made of a single thread formed into a cylindrical tube.  They were handmade by a process then called tatting and now known as crocheting.  Unlike knitting, which uses two threads and two needles, crocheting only requires one tool, called a hook.  The hook size is scaled to the thread diameter.  In its simplest execution, the process produces a chain-like, continuous series of interlocking loops.  Lace, circular doilies, and rectangular antimacassars were made by creatively interconnecting the chain to form symmetrical patterns.   In the “men’s work – women’s work” divide, tatting fell under the women’s craft and so the products were always useful at home.
Grandma Pickering taught me to tat chains as a preschooler which kept me non-kinetic and silent as I marveled at the ever longer creations while I tried to out-do myself day after day.
 
To make a tube, a mandrill or tool is used with the hook.  The tool consists of a tube with projection pins at one end.  The diameter of the stocking (hose and the frequency of pins controls the symmetry and mesh size.  For each pair of stockings an appropriate length was cut off and knotted to prevent unraveling.  The toe was neatly tied off and a garter, i.e. non-stretchable holder, was sewn or tatted to the top. 
 
By grammar school, I made my own tube tool with a wooden thread spool and headless brads.  I don’t remember the hook, but I suspect it was made from a piece of wire hanger.
The larger ID reactors that Pickering Laboratories offers are made like stockings.  The mandrill has four pins.  The misnomer is that our literature calls them “knitted” because that is the most common description in print and conversation in our industry.  Describing them properly would only create a lot of idle questions.  The necessity for the crocheting is to minimize band spreading.  The post-column reaction occurs after the separation is complete, so when the peaks enter the reactor they are as far apart as they are going to be.  The torturous path eliminates the band spreading of longitudinal mixing by replacing it with radial mixing.

Pickering Laboratories to introduce new and updated products and applications at PITTCON

By Mike Gottschalk

PITTCON 2011 – Atlanta, Georgia:

Pickering Laboratories is building on the success of the LCTech product line with the introduction of the new GPC VARIO III, a fast and flexible instrument for Gel permeation chromatography (GPC) and upgradeable for automated sample preparation using SPE.  
The GPC VARIO III is completely re-designed to optimize every component of XYZ Robot arm technology for faster processing and feature-rich flexibility. Highlighted is the innovative arm technology that handles the processing of samples.
The integrated software allows for easy setup with drag and drop icons for even complex multi-step processes for volumes of 1mL to 1Liter . The modular design enables processing scalability and flexibility to standard columns, bottle and vial sizes.
Another GPC instrument, GPC Quattro will be shown. This popular 4 column GPC is designed for concurrent operation of 4 columns providing the faster throughput and flexible programming. 
For Post-Column applications the new Pinnacle PCX Sigma series instrument featuring faster Amino Acid Analysis and new software features is being introduced as an update to our line of derivatization instruments.  The small yet powerful UVE photochemical reactor for Aflatoxin analysis will also be shown.
Pickering Laboratories will be introducing new post-column methods for Hexavalent Chromium (Chrom-6), Aflatoxin in herbal products. As part of the AFFCO and AOAC lab committee collaboration Pickering Labs developed our new method for the effective analysis of Sugars in feeds with existing and additive sugars.
With increasing interest in Chromium 6 in drinking water this year,  Pickering Laboratories is publishing an updated Chromium 6 method demonstrating definitive yet easy analysis.
Pickering Lab’s technical liaison director Laszlo Torma is a member of the American Herbal Products Association (AHPA) laboratory committee. The work of the committee and collaborating with AOAC has resulted in new methods for analysis of Mycotoxins in many herbal products including ginger, ginseng, Echinacea.
Come to Booth 1767 at Pittcon to see and hear about the exciting work going on at Pickering Laboratories.

Pickering Laboratories Introduces Key Products to Herbal Supplements Market

By Mike Gottschalk

The Supplyside West Conference in Las Vegas, Nevada October 19-23, is a very important Herbal Supplement Industry event. It provides important educational and networking opportunities to this $29 billion market. Since the FDA sent out required current good manufacturing practices (cGMP) in 2007, the Herbal Supplement producers are working to meet the new requirements before the FDA audits. These regulations are intended to insure the quality, purity and safety of the Herbal Supplement products available today. Pickering Laboratories had a booth at the show to assist the producers and laboratories with the instrumentation, chemistry, methods, and support for the analysis and clean-up of samples for Amino Acids, Aflatoxins, Carbamate pesticides, Glyphosate Herbicides, and 23 other methods.

Click on the links to see our Latest Method Abstracts, introduced at the show:
1) MA 215: Clean-up and Determination of Alfatoxins in Peanuts and Peanut Butter 

2) MA 218: Clean-up and Analysis of Aflatoxins and Ochratoxin A in Herbs and Spices 


The annual meeting of the AOAC International in Orlando, Florida on September 20-25, also had a strong emphasis on Herbal Supplements testing. The AOAC organization is central to FDA efforts to provide analytical structure to testing methods for this newly regulated industry. Pickering Laboratories participated in the AOAC sponsored Single Laboratory Validation of Multi-residue Mycotoxin Analysis in Corn. For this work, Pickering Laboratories was awarded the “Single Lab Validation of the Year”. This pivotal work in the analysis of Mycotoxins continues in Herbal Supplements as well as agricultural products.

Send us an email to support@pickeringlabs.com to request a copy of our poster: “Clean-up and Determination of Alfatoxins in Peanuts and Peanut” from the AOAC show.

Our next show is Pittcon 2011 on March 13-18 in Atlanta, Georgia.

See you there!

ACIL Annual Meeting, San Diego, California

The American Council of Independent Laboratories (ACIL) show in San Diego, California on October 9-12, was a new opportunity for Pickering Laboratories to introduce ourselves to the principals of these independent laboratories during their annual networking meeting.

The meeting was a great opportunity to visit with existing customers, but also to make new contacts in the Environmental testing industry. At the meeting we had information on our mainstay applications and also presented our new GPC Cleanup Instruments and other new products to prospective customers.

Rebecca Smith reports that the meeting was a success in terms of networking, scientific and educational talks.

Our new Gel Permeation Chromatography (GPC) line continues to perform well. We have both automated and manual GPC cleanup systems and we also have systems that include concentration & solvent exchange. Sample cleanup using GPC is especially useful for fatty matrices, but also perfect for vegetable matter and spices, as well as soil & waste water.

Our next show is Pittcon 2011 on March 13-18 in Atlanta, Georgia.

You can read more about the ACIL at their website: www.acil.org

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