Category Archives: pickering laboratories

AOAC, HPLC, pickering laboratories, pinnacle pcx, post-column derivatization

Polyether Antibiotics in Animal Feed

Our updated Method Abstract 264 describes the analysis of Monensin, Salinomycin, Narasin, & Lasalocid in Animal Feeds.

Polyether Antibiotics are commonly used for preventing coccidiosis and other infections in poultry and for improving feed efficiency for beef cattle and swine. The use of Polyether Antibiotics is strictly regulated, with only specific ionophores approved for use in feeds intended for different animals.

Analysis of Polyether Antibiotics by HPLC with post-column derivatization and UV/Vis detection has been proven to successfully identify and quantify Monensin, Narasin and Salinomycin in medicated feeds, supplements and premixes as well as to determine trace contamination levels in non-medicated feeds [1, 2].

Post-column derivatization of Polyether Antibiotics is done using highly acidic Vanillin or DMAB reagents. The Pinnacle PCX derivatization system (Pickering Laboratories, Inc.) has an inert flow path and automated system wash capabilities that make it uniquely suitable for handling corrosive reagents. The two-pump system is recommended to extend reagent stability, but the single-pump system for this application is also available.

Adding a Fluorescence detector to the instrumentation allows for using the same extraction procedure and HPLC conditions to also determine Lasalocid, which doesn’t require post-column derivatization.

Chromatograms of Polyether AntibioticsMETHOD
Sample Preparation
To 25 g of finely ground feed sample, add 100 mL of extraction solution (90% Methanol – 10% water). Shake for 1 hour at high speed using a mechanical shaker. Let the solids settle and filter an aliquot of the extract for injection. Dilute with extraction solution if needed to fit the calibration curve. Use a 2.5 g portion when testing premixes.

Analytical conditions
Analytical Column: Polyether Column, C18, 4.6 x 250 mm, Catalog No 2381750
Temperature: 40 ºC
Flow Rate: 0.7 mL/min
Mobile Phase: 90% Methanol, 10% of 5% Acetic Acid solution in water, isocratic
Injection volume: 20 μL

Post-Column Conditions
Post-column System: Pinnacle PCX
Reactor Volume: 1.4 mL
Reactor Temperature: 90 °C
Reagent 1: Concentrated Sulfuric acid / Methanol (4:96 v/v)
Reagent 2: 60 g of Vanillin in 950 mL of Methanol
Reagent Flow Rate: 0.3 mL/min
Detection: UV/VIS 570 nm (for Lasalocid – FLD, Ex. 322 nm, Em. 370 nm)

Conclusion
Analysis of Polyether Antibiotics by HPLC with Post-column derivatization is a robust and sensitive method that utilizes standard equipment and could easily be adopted by testing laboratories. It allows for testing of different ionophores at wide range of concentrations,
including at trace levels. Using Pinnacle PCX post-column derivatization system, factory configured for the analysis, guarantees stable and reproducible results.

The full application note as well as our complete Product Catalog can be downloaded from our website: www.pickeringlabs.com

table for polyether antibiotics

aflatoxin, Amino Acid Analysis, amino acids, antioxidants, artificial perspiration, clean-up, deoxynivalenol, freestyle, glyphosate, GPC, immunoaffinity cleanup, mycotoxin, natural toxins, New Products, pickering, pickering laboratories, pinnacle pcx, post-column derivatization, Uncategorized

2013 Pickering Laboratories North American Catalog

Our latest Catalog for North America is now available!

Click on the link to download the latest product Catalog from Pickering Laboratories, Inc.

Pickering Catalog: http://pickeringlabs-retentiontimes.com/wp-content/uploads/2013/08/2013_PickeringLabs_Catalog_NorthAmerica_LowRes.pdf

Inside our catalog you will find a complete product listing for all instruments and consumables we currently have available. From Sample Cleanup to Post-Column Derivatization, to artificial Perspiration and Saliva, we hope you find something you will find useful!

elisa, ergot alkaloid, lctech, mycotoxin, natural toxins, pickering laboratories

Analysis of Total Ergot Alkaloid Amount in Various Grain Samples by ELISA

By Dr. Frederik Wuppermann and Dr. Uwe Aulwurm

Introduction:

Ergot alkaloids are mycotoxins produced by fungi (Claviceps sp.) on various grain species with a highly toxic impact on the health of consumers (Figure 1). The toxins provoke symptoms summarized as ergotism.

ergot wheat

Figure 1: Sclerotia grown on crop

The toxins are characterized by two different isomers, which occur under different pH conditions, they are named –ines and –inines. The main toxins found are ergocristine, -inine, ergometrine, -inine, ergosine, -inine, ergocryptine, -inine, ergotamine, -inine, ergocornine, -inine. The assessment of toxin amount becomes necessary due to the toxic effects of ergot alkaloids. For this purpose an ELISA was developed to detect all ergot alkaloids in various crop material and the detected amounts of ergot alkaloids were correlated with LC-MS data.

 

 

Method

ergoread quick method
Figure 2.
ELISA procedure

The sample is extracted by 40/60 methanol / 0.25% phosphoric acid as described by Ware et al. 2000. After centrifugation the sample was diluted with sample dilution buffer and filtered again. The filtered sample was applied in the ELISA plate and compared with a standard solution (enclosed in the ErgoREAD kit). The enzyme immune reaction is performed as depicted in Figure 2.

 

 

Results:

Analysis of wheat samples:

analysis of wheat

 Analysis of Rye Samples:

analysis of rye

Comparative Analysis of Naturally Contaminated Samples:

The samples showed good correlation between 0 to 10 ppm, indicating that the ELISA is suitable for the screening of various crop material for the presence of ergot alkaloids. The partially over quantification in the comparative analysis could be due to the cross reactivity of the ELISA against various ergot alkaloids which were not monitored by the LC-MS or HPLC analysis. comparative analysis of naturally contaminated samples

Figure 3 cross reactivity of ErgoREADThe ELISA shows significant cross reactivity against various ergot alkaloids e.g. ergonovin (ergometrine or ergocristine) and can be used to determine the qualitative stuatus of a crop sample concernig the sum of ergot alkaloids.

 Conclusion:

The ErgoREAD ELISA is an appropriate tool for screening wheat, rye and triticale samples for presence of ergot alkaloids. The range of measurement is from 0 to 5 ppm. Due to the readout as the sum of all reactive ergot alkaloids, the cutoff for critical samples is 0.4 ppm. All shown ELISA samples are correlated with HPLC. The total amount of samples which need to undergo LC-MS analysis could be dramatically reduced.

More information about this kit and other Mycotoxin analysis products can be found on LCTech’s Website. The original poster can be downloaded here.

Pickering Laboratories is proud to bet the distributor for LCTech in North America. For more information about our long-time relationship with LCTech, check out our blog entry on Pickering’s Company & Product Offerings in 2013.

 

 

AcceCLEAN, aflatoxin, amino acid, Amino Acid Analysis, amino acids, antioxidants, AOAC, AOAC's Laboratory of the Year Award, artificial perspiration, carbamate, Chromatography, clean-up, column, deoxynivalenol, detector, dietary supplements, DON, Dr. Pickering, elisa, eluvac, ergot alkaloid, freestyle, GARD, glyphosate, GPC, Guard, HPLC, immunoaffinity cleanup, Multi-residue Mycotoxin Analysis, mycotoxin, natural toxins, New Products, Ninhydrin, ochratoxin, paralytic shellfish toxin, Physiological Fluids, pickering laboratories, pinnacle, pinnacle pcx, Post-column, post-column derivatization, psp, sweat, syringe pump, Trione, UVE, vector

Pickering Laboratories in 2013

1 Comment

By Wendy Rasmussen

In recent years, we have released several new products and applications, and with still more on the horizon, it occurred to me that now would be a great time to summarize the Pickering of today – our mindset and our wide variety of products & applications.

Acai Berries
Acai Berries

No longer are we simply the “Post-Column Company”. We are the “Automated-Sample Antioxidants” company.  Think of us as the new “super fruit.” The Acai berry, or perhaps the new Chia Seeds (incidentally, we do have a post-column application for the identification & quantitation of  Antioxidants in a variety of matrices).

We are still very active, and we as a company plan to be here for many years to come. We are still the company founded on chemistry and a desire to to teach, to spread our technical expertise, to support our customers.

It’s been a few years now since Pickering began distributing and supporting our LCTech Product line.  The products have shown an ever increasing interest here in the US and in Canada (our official Sales Territory for this product line). We are very proud to offer these products and we hope we can develop it further in the future.

Historically, we have provided the back-end of an analysis (post-column derivatization). Nowadays, we can provide the front-end of analysis as well (the sample-cleanup).

In thinking about our product offerings, I realized that a simple list does not effectively show the scope of the products we have to offer in 2013 – primarily because we have a lot of overlap between products and product lines.  We’re not a vertical company in that regard.  I suppose one could say our product offerings are more circular in that many do not fall into a single distinct category.  I am a very visual person, and for me, a Venn diagram and our overall “product scale” really helped to understand and clarify our products:

Venn Diagram of Pickering Laboratories
Venn Diagram of Pickering Laboratories
General "Product Scale" for Pickering Offerings
General “Product Scale” for Pickering Offerings
For those of who like lists, you can find one Here, on Pickering’s website, and on LCTech’s Website

For any Questions, please feel free to contact us:

Pickering Laboratories, Inc.
Mountain View, California
Email: sales@pickeringlabs.com
Phone: (direct) 650-694-6700 or (toll-free) 800-654-3330

 

Image of Acai Berries:  http://acaiberryeducation.com/

carbamate, Chromatography Quiz, pickering laboratories, post-column derivatization

Chromatography Quiz No. 13

Chromatography Quiz #12 Results

We would like to congratulate our grand prize winners of our last newsletter’s Amino Acid Analysis Chromatography Quiz: Luiz Paulo Mousinho from Chemetric in Brazil, Helene Lachance from Shur-Gain Nutreco in Canada, and Narjes Ghafoori from the LA County Environmental Toxicology Laboratory!!!

They have each won and will be receiving: a $100 gift card from Amazon.com!  We would like to thank all of you for your submissions.

The correct answer for the modified Amino Acids chromatogram: the back pressure regulator on the outlet of the detector stopped functioning properly.  This was indeed another hardware troubleshooting quiz!  The pattern of noise seen in the customer’s baseline is characteristic to this problem, and a new back pressure regulator eliminated the noise.

Thank you!
Pickering Labs

Chromatography Quiz #13:
Identify the error made when running the Carbamate chromatogram below and win a prize!  Simply email your answer as well as your full contact information to Rebecca at rlsmith@pickeringlabs.com by August 30, 2013 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).

Carbamate Analysis for US EPA Method 531.1

Pickering Standard: 1700-0063 Carbamate Test Mixture, 2.5 µg/mL, 10 µL injection

Pickering Column: 1846250 Carbamate Column, C18, 4.6 x 250 mm

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

Column Temperature: 42 °C

Flow rate: 1 mL/min

Eluent Gradient:

TIME

WATER

MeOH %

0

85

15

1

85

15

44

25

75

44.1

0

100

49

0

100

49.1

85

15

57

85

15

 

Post-column conditions:

Reagent 1: Hydrolysis reagent CB130

Reagent 2: 100 mg of OPA, 2 g Thiofluor™ in 950 mL of CB910

Reactor 1: 100 °C, 0.5 mL

Reactor 2: ambient. 0.1 mL

Reagent flow rates: 0.3 mL/min

Detection: Fluorometer ex 330 nm, em 465 nm

Troubleshooting Chromatogram:

Troubleshooting chromatogram_CarbamateReference Chromatogram:

Reference chromatogram_Carbamate

aflatoxin, Amino Acid Analysis, carbamate, chromatographic specialties, Chromatography, clean-up, eluvac, freestyle, glyphosate, GPC, herbal products, HPLC, immunoaffinity cleanup, lctech, Multi-residue Mycotoxin Analysis, mycotoxin, natural products, natural toxins, New Products, Ninhydrin, ochratoxin, pickering laboratories, pinnacle pcx, Pittcon, post-column derivatization, spe

Pickering Exhibits at Pittcon 2013

This year’s Pittcon was held in Philadelphia, Pennsylvania from March 17-21, 2013.

view of philly from the museum On display were Pinnacle PCX, EluVAC, and a video of the FREESTYLE Automated Sample Preparation Instrument.  The video was a new technique for us, and it was well received.

The video in our booth was a combination of the separate videos for each module of the FREESTYLE Automated Sample Preparation Instrument. You can view the originals here (they are very informative, and we highly recommend them): FREESTYLE VIDEOS

Wendy, Mike and David enjoyed visiting with existing and future customers, as well as our distributors from around the world, including our Canadian distributor, Chromatographic Specialties.

Before the show opened, we had the opportunity to explore the city.  Philadelphia is one of our oldest cities and is full of history and landmarks. Some of this editor’s favorites include Independence Hall and the surrounding neighborhoods, and the Art Museum (see more below).  On this trip, we explored Reading Terminal Market, and sampled that famous cuisine, the Philly Cheese steak Sandwich. I’m told it is not truly a Philly Steak sandwich unless you have it with Cheez Whiz. Any type of real cheese doesn’t count. I made that mistake on my first trip to Philadelphia, and the man behind the counter let me know it!  I wasn’t about to make that mistake again:

philly cheesesteak

The Philadelphia Museum of Art is known for its amazing collection of artwork (viewed on a previous visit), but is also made famous by the scene of Sylvester Stallone running up the stairs in the movie Rocky.  Since the author of this entry happened to be training for a race, she decided that a little cold wasn’t going to stop her. So she put on her iPod (Rocky Theme playing, of course), and ran from the hotel to the top of the steps and back (total distance: about 2.8miles).

view from the bottom

wendy philly top of steps

wendy rockyOn the return to the hotel, I came across a version of the LOVE sculpture, by American Artist Robert Indiana. I always thought it was was much bigger…

love sculpture

 

For those of you interested in learning more about the sculpture, click HERE

If you’re ever in Philadelphia, the Philadelphia Museum of Art is definitely worth a visit.

But if you can’t make the trip to Philadelphia, you could also stay home and watch Rocky…

antioxidants, AOAC, herbal products, mycotoxin, natural products, natural toxins, pickering laboratories, supplyside

Pickering exhibits in Las Vegas

-By Mike Gottschalk

Las Vegas, Nevada – Oct. 1 – 5 was the site of the AOAC international show this year.  Pickering Laboratories participated as usual in this important International event. “We see many of our customers and distributors from all over the world at this show” said Wendy Rasmussen, sales manager Pickering Laboratories. “We get to show our new products and catch up with them with new developments in their business.”

Pickering Laboratories presented Posters of our new applications Chrome VI and Antioxidants in foods. The herbal supplement market is a growing market and with FDA guidance, more concerned with testing for quality in their products. “We continue to develop methods in matrices important to this market including the antioxidants, Aflatoxins, Amino Acids and others”  said Laszlo Torma, technical liaison for Pickering Laboratories.

The AOAC international show enables laboratories and suppliers to be involved in the mission of creating analytical methods for today’s most pressing testing challenges. Pickering Laboratories is an award winning member of several committees and laboratory collaborations to further the goal of analytical excellence.

Las Vegas, Nevada – Nov. 6-9 – Yes! Las Vegas Again! This time for the annual Supply Side West show.  1,800 vendors and 30,000 participants meet to network and explore resources in this, the largest gathering of Herbal supplement suppliers and vendors.  Now that the FDA enforcements are increasing, many Herbal supplement manufacturers are working hard to improve their analytical testing capabilities and Pickering Laboratories is there to help.  “With several methods for herbal supplement testing and extensive experience in the food safety industry we can offer experience and laboratory equipment support to the herbal supplement manufactures” – said Mike Gottschalk, VP Marketing, Pickering Laboratories.

Laszlo Torma enjoys the sights and sounds of “Venice”

Pickering Laboratories is a member of the “American Herbal Products Association” and member of the Laboratories Methods Committee for AHPA. The collaboration with AHPA and the Supply Side West show have provided valuable insight to the needs of the Supplement community and the unique capabilities Pickering Laboratories can offer this market.