Pickering Laboratories

NEW Amino Acid method: Oxidized Feeds in 30 minutes

Dear Valued Customer,
We are pleased to announce the new 30 minutes Oxidized Feed method. This method uses the new fast sodium column 1154110T and utilizes the column temperature gradient with the Pinnacle PCX. Because this method uses a column temperature gradient, it is important to note that the method is not compatible for Vector or PCX5200 users.

Peak Identification
1. Cysteic Acid
2. Methionine Sulfone
3. Aspartic Acid
4. Threonine
5. Serine
6. Glutamic Acid
7. Proline
8. Glycine
9. Alanine
10. Valine
11. Isoleucine
12. Leucine
13. Phenylalanine
14. Lysine
15. Histidine
16. Ammonia
17. Arginine

Kits are available and include the following:

0352-0020 30 minute Oxidized Feed Kit – T100C
1154110T Qty 1 Column, Fast Sodium 4.6x110mm (includes 1700-070 Test Mix)
1700-3102 Qty 1 Kit, GARD Holder and 2 Cation GARD
1700-0155 Qty 1 Cal Standard, Feed Hydrolysate
Na220 Qty 1 Sodium Diluent, pH 2.20 4x250mL
Na270 Qty 1 Sodium Eluent, pH 2.80 4x950mL
Na740 Qty 1 Sodium Eluent, pH 7.40 4x950mL
RG011 Qty 1 Sodium Column Regenerant 4x950mL
T100C Qty 1 TRIONE, Ninhydrin Reagent 4x950mL

0352-0021 30 minute Oxidized Feed Kit – T200
1154110T Qty 1 Column, Fast Sodium 4.6x110mm (includes 1700-070 Test Mix)
1700-3102 Qty 1 Kit, GARD Holder and 2 Cation GARD
1700-0155 Qty 1 Cal Standard, Feed Hydrolysate
Na220 Qty 1 Sodium Diluent, pH 2.20 4x250mL
Na270 Qty 1 Sodium Eluent, pH 2.80 4x950mL
Na740 Qty 1 Sodium Eluent, pH 7.40 4x950mL
RG011 Qty 1 Sodium Column Regenerant 4x950mL
T200 Qty 1 TRIONE, Ninhydrin Reagent 2 part

0352-0022 30 minute Oxidized Feed Kit – O120
1154110T Qty 1 Column, Fast Sodium 4.6x110mm (includes 1700-070 Test Mix)
1700-3102 Qty 1 Kit, GARD Holder and 2 Cation GARD
1700-0155 Qty 1 Cal Standard, Feed Hydrolysate
Na220 Qty 1 Sodium Diluent, pH 2.20 4x250mL
Na270 Qty 1 Sodium Eluent, pH 2.80 4x950mL
Na740 Qty 1 Sodium Eluent, pH 7.40 4x950mL
RG011 Qty 1 Sodium Column Regenerant 4x950mL
O120 Qty 1 OPA, 5g
OD104 Qty 1 OPA Diluent 4x950mL
3700-2000 Qty 2 Thiofluor, 10g


David Mazawa

Technical Support Chemist
Pickering Laboratories, Inc.
1280 Space Park Way
Mountain View, California 94043 USA
Phone: 650-694-6700, ext. 710
Toll Free: 800-654-3330, ext. 710

A Brief Report on the European Pesticide Residue Workshop in Strasbourg, France

By Laszlo Torma
The 8th European Pesticide Residue Workshop (EPRW 2010) was held in Strasbourg, FR on June 20-24, 2010. As usual, EPRW 2010 was a great success and it was a productive and worthwhile meeting.

First, I would like to share a little information about Strasbourg. The city is the capital of region which was part of the Holy Roman Empire and later annexed by France. In more recent history, Alsace changed hands four times between France and Germany in 75 years. Although the historical language of Alsace is Alsatian, a Germanic language, today most Alsatians speak French and only about 40% of the adult population is fluent in Alsatians. Strasbourg is the seat of several European Institution such as the European Parliament, the Council of Europe (with its European Court of Human Rights) and others.

Back to the meeting; EPRW meets every 2 years and in my opinion, it gets better and larger each time. In spite of the global economic down turn, there were about 500 participant and 30 exhibitors representing all the continents. The Scientific Organizing Committee has assembled a great program, including 29 oral presentations, more than 200 posters and a number of vendor sessions. Scientists from all over the world were represented and participated in various discussions to exchange new ideas in the area of pesticide regulations, residue monitoring, new analytical techniques and methodology. I enjoyed the high quality posters that have been presented. These posters demonstrated the desire of many scientists to share their practical and fundamental know how with the participant during the workshop. And last but certainly not least, I had the opportunity to work with our European distributor, LCTech from Germany and to visit with our mutual customers.

Pickering Laboratories at the Florida Pesticide Residue Workshop

By Wendy Rasmussen

Last month we participated in the Florida Pesticide Residue Workshop, held in St. Pete’s Beach in Florida from July 18-21. It was a very interesting meeting from many aspects: talks, posters, mix of attendees and exhibitors, current topics. There were talks on mycotoxins and veterinary drugs as well as policy and risk assessment.

Pickering presented a Vendor breakfast session on Wednesday July 21, titled “Keys to an Analytical Method: Focus on Mycotoxins” We decided to highlight our Mycotoxin analysis product line which we are distributing from our German partners, LCTech GmbH

The weather was unusually cool for Florida in July, hovering in the mid-90s (35°C). The water temperature in the Gulf was surprisingly refreshing at “only” 89°F (32°C). The usual thunderstorms were present, although fewer in number. Mother Nature provided us with some very impressive lightning storms just off shore in the evenings.

The meeting was much larger this year, both in terms of attendance and exhibitors. Not only were there more attendees, but there was a very large number of First-time attendees, as well as a greater contingency of international attendees from Europe, Asia, Australia, and South America. There were 226 attendees and 25 exhibiting companies.

One of the hot topics of discussion at the meeting was the Deepwater Horizon spill in the Gulf. No oil
has reached that part of the Florida coast, and so the beaches were open, but inside there was much debate about the testing of the seafood for PAHs, the cleanup of the spill, and the environmental impact, both on marine human life. There was a great deal of discussion about using the NOAA method for PAHs (which involves GPC Cleanup), as well as testing for the alkyl homologs present in the oil and potential screening methods to speed up the analysis time.

GPC cleanup remains very effective at cleaning up fatty and complex matrices, and it’s still part of the official methods. GPC Quattro would be an excellent choice for this. With 4 individual channels, each with their own pump and lines, and with rugged, easily repackable columns, a lab would get 4 times the productivity of a single column system: GPC Quattro

Links for info on the Gulf:
There is an abundance of websites, news, and general information about the oil spill. Here are a few links I found to be interesting:

The FDA has approved an HPLC-FLD screening method for the PAHs, which will still need confirmatory testing, but this will decrease the initial testing time down from 4-5 days to 48hrs.
For FDA’s latest updates: http://www.fda.gov/Food/ucm210970.htm

It’s been proposed that we should be looking at Alkyl Homologs of PAHs. Ed Overton gives a pretty good overview of these compounds and the composition of oil spills in general: Overton perspective

Restek recently analyzed some of the oil via GCxGC-TOFMS: ChromaBLOGraphy

(This is not meant to be a comprehensive list, nor is there any endorsement intended or implied)

Del Rio, Texas

By Michael Pickering

While in graduate school at the Oregon Graduate Center, a private technical school with no undergraduate program, my advisor, G. Doyle Daves was awarded a grant to elucidate plant toxins. The plant, Karwinskia humboldtiana, known by Texas ranchers as “coyotillo,” has toxins in its ball-bearing like seed that cause rising paralysis
from the hind quarters to eventual death. Although human poisoning is extremely rare, the oldest documented poisoning is a conquistador soldier who was hungry and had strong jaws to crush the seeds.

Since I was already into plant secondary metabolites due to my M.S. research, I eagerly volunteered to go to Del Rio for the first harvest. Del Rio is a small town on the Rio Grande about an hour car drive southwest of the San Antonio airport. A bridge walk across the river gets you into the thriving village (as in mostly well-maintained dirt roads) of Ciudad Acuña, Mexico. It was attractive and friendly. Each morning I would walk over to get a pan dulce for my morning coffee; I then had lunch in Del Rio and then back to Mexico for dinner. The most striking feature of Acuña is a thin, Eiffel-like 300-foot metal broadcasting antenna stand. This is XERB’s continent-spanning 250,000 watt broadcasting transmitter – illegal a few feet from where it stands, made famous by Wolfman Jack. (¿Te acuerdas de una época en que se pensaba que los Americanos eran ingeniosos solucionarios de problemas?)

The regional climate is semi-arid. The topography is the largest area of flat ground I have ever seen. The surface appeared to be very small gravel or coarse sand. Flora is sparse. The largest visible plant is the coyotillo at 4-6 feet, which evenly dotted the available view. The only other noticeable plant was a 2-inch very sparse dry grass.

Permission to collect plant material was arranged by the USDA soil conservationists who had an office in town. Each day they would introduce me to the host ranch owners where I was going to collect. Much friendly teasing about this young Oregonian’s coon-like behavior, taking poison berries home, was endured during introductions. The ranches were 100,000+ acres of cattle and sheep. The ranchers’ grandfathers had been shepherds; their fathers became cattlemen when synthetics undermined the market for wool and cotton. The source of livestock was Mexico via rail. The cattle looked like starving animals when they arrived to be put to graze and become normal looking animals when they were wholesaled to feed lots in the northern states. That sparse grass has to be high in protein – not only do the livestock prosper, the land teems with deer and other vegetarian wildlife. Because of the size of the ranches, an important part of their revenue is selling hunting packages to corporations in Louisiana and Texas. After all, they have well-maintained bunkhouses and appropriately sized kitchens and dining areas. The locals don’t hunt deer; they all have a pen of small ‘Mexican” goats at home for the table.

Still in the field but back to the berry: it is the color of a small dark blueberry, with a thin coating of flesh over a spherical seed. The ring-tailed raccoon knows not to crush the seeds when feeding and thus is the planter that adorns the landscape with seeds and appropriate fertilizer. The leaves and stems are non-toxic and as such are reliable and bountiful resources for browsers.

Unfortunately my visit there followed a major drought. The plants were suffering since rain is the only habitat irrigation. Visually, they sorted into two categories: 1) bushes with sparse berries and almost no leaves, and 2) lush, green bushes with no berries. We knew that the toxin was only in the hard seed, which was most of the mass of the berry, so we wanted to maximize the collection of the berries.

The collection period was five days. The plan was to collect berries three to four days, and to collect leaves otherwise. In anticipation of leaf collection, I went to a local coffee roaster and bought some burlap bean shipping bags. Also on hand were a curved upholstery needle, appropriate twine, and proper shipping tags for rail cargo.

Each morning I would start harvesting berries until the territory got so big, i.e. distance from the car, that I would then begin stuffing leaves into bags, i.e. very little walking. Many stomped bags of leaves were shipped by rail, and the drought-impacted, meager berry harvest was no more than a carry-on for the flight home.

When the ranchers brought in 100 head of cattle from Mexico, they lost one to two steers to the toxin. When they brought in 100 sheep, they lost two to four. The toxins are a group of four red, closely related compounds. For more information, see Doyle’s paper in the Journal of the American Chemical Society: “Toxins Causing Noninflammatory Paralytic Neuronopathy, Isolation and Structure Elucidation,” August 1975, pages 4985-4990.

Editor’s Note:
I was curious as to the location and look of Del Rio and Ciudad Acuña. For anybody interested in Geography, check out these links:

Photos from the Universidad Autonoma de Ciudad Juarez:

And also from the TX Dept of Transportation: http://www.txdot.gov/project_information/projects/border_crossing/delrio.htm

Karwinskiana photo: http://www.swsbm.com/Images/New2005/Karwinskia_humboldtiana-2.jpg

Sigma Series Pinnacle Control Software

By David Mazawa

You may have noticed something different about the Pinnacle. That is because the new Pinnacle Sigma series started shipping out mid June. Some improvements include fully ROHS compliant components, power cooling, USB connection, log file expansion, PEEK front end for reagent pumps, and lighter parts. It is important to note that new Pinnacle Control Software has been updated to support some of the new features.

Before installing the new software, make sure to export your Methods and Sequences. This will create a back up of all your Methods and Sequences. It is possible that your old Methods and Sequences will not transfer after installation of the new software. If this is the case, import your backup file.

You will notice that you need to install drivers with the new Pinnacle Control Software. The drivers are required to communicate with the USB port of the Sigma Series Pinnacle. We have replaced the RS-232 connection with USB. Make sure you follow the instructions included with the Pinnacle Control Software Installation CD.

After you have installed the new Pinnacle Control Software, make sure you double check the instrument configuration. It is possible that the default configuration of “No Connection to HPLC” will be loaded. After your methods and sequences are imported and your configuration is correct, you are ready to use the new Pinnacle Control Software.

The new Pinnacle Control Software includes pressure tests. These pressure tests should be used after a PM or when pump or valve seals have been replaced. You can pressure test individual pumps or pressure test the entire system. Make sure to follow the instructions presented by the Pinnacle Control Software. These tests can be found under Instrument then Maintenance.

The Pinnacle Control Software has expanded the log files. An extra day of data is collected and more detail is collected per log file. This will greatly help Pickering Laboratories Technical Support troubleshoot any problems you may have in the future.

Please email or call Pickering Laboratories Support with any questions.

support@pickeringlabs.com / (650) 694-7700 / (800) 654-3330

David Mazawa

Technical Support Chemist


(650) 694-6700 x 710

Pickering Expands into the OEM Pump Market!

By Mike Gottschalk

Pickering Laboratories has made available the Pinnacle PCX syringe pump for OEM applications. The pump is the heart of the successful Pinnacle PCX instrument. “This syringe pump’s service record and performance are truly remarkable. We designed it for long life and exacting specifications; now six years later and a thousand working units in the field we are very confident this pump will be successful in other applications”, said Michael Pickering.

When the Pinnacle PCX was designed a suitable pump could not be found so the design of a perfect syringe pump was begun. The results are a very precise, pulse free, and inert pump rugged and reliable enough for our analytical chemical instrument. The current specifications are an alumina ceramic cylinder with PEEK for inert flow path, a 70 ml volume cylinder, low flow rates range of 30µL/min – 1500µL/min, at pressures of 300 – 500 psi.

Of all the syringe pumps available today our pump is unique in its pressure range and absolute inert materials. These features will be useful in industrial fluid delivery applications and we will begin marketing to the large industrial equipment market. We have engaged with Globalspec to help us introduce this product. Globalspec is the leading specialized vertical search company serving the engineering, manufacturing and related scientific and technical market segments.

For more information on the OEM Syringe pump:

Chromatography Quiz No. 4

Chromatography Quiz #3 Results
Congratulations to the grand prize winners of our last newsletter’s Glyphosate Chromatography Quiz: Jim Balk from Nebraska DHHS Public Health Environmental Laboratory, Matthew Hartz and Keena Njoroge from Underwriters Laboratories, and Narjes Ghafoori from the County of Los Angeles Environmental Toxicology Laboratory! They have won, and will shortly be receiving from Apple.com, a new iPod Shuffle! Additionally, for this third quiz all of our participants will be receiving a $10 gift card from iTunes. Thank you all for your submissions!

The correct answer for the modified Glyphosate chromatogram: the Glyphosate ‘doublet’ is caused by injecting a sample at basic pH. An improperly buffered sample extract at a large injection volume will not mix with the mobile phase sufficiently to create the acidic pH necessary for Glyphosate to be at the proper single charge state, impacting the interaction between Glyphosate and the active
sites on the column resin. Adding a couple drops of Restore TM(pH 1.3) to the sample before injection will eliminate the ‘doublet’ and return proper peak shape.
Thank you!
Pickering Labs

Chromatography Quiz #4:
Identify the error made when running the Amino Acids chromatogram below and win a prize! Simply email your answer as well as your full contact information to email Rebecca Smith by September 30th in order to win. You will receive email confirmation when your submission is received, and the troubleshooting answer and winner congratulations will be published in the next issue (to be anonymous, please notify Rebecca in submission).

Amino Acid Analysis of Physiological Fluids
Pickering Standard: 011006P Native Sample Standard 0.25 µmole/mL, 10 µL injection
Pickering Column: 0354100T High Efficiency Lithium Cation-exchange Column, 4.0 x 100 mm
Pickering Guard Column: 0352020, 2.0 X 20 mm

Normal Operating Conditions: (for reference only, condition changes may be reflected in chromatogram)

Column Temperature: 37 °C
Flow rate: 0.35 mL/min

Eluent Gradient:










Post-column conditions for amino acid analysis:
Reagent 1: Trione


Reactor 1: 130 °C, 0.5 mL
Reagent flow rate: 0.3 mL/min

Detection: UV-Vis Detector: 570 nm for primary amino acids, 440 nm for secondary amino acids

Post-column conditions for amino acid analysis
You can find an example of a good chromatogram page on our website.  

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