Chromatography Quiz #27: Only AMPA

Chromatography Quiz #26: Shifting Retention Times – Carbamates — Results

Pickering Labs would like to congratulate the winners of our last newsletter’s Shifting Retention Times–Carbamates Quiz: David Green from Pepperdine University, Jeff Fan from Cumberland Valley Analytical Services, Karissa Scroggins from North Coast Laboratories, Jim Balk from Nebraska DHHS Public Health Environmental Laboratory, Narjes Ghafoori from LA County Agricultural Commissioner Weights & Measure Environmental Toxicology Lab, Tom Schneider from Suffolk County Water Authority, and Ms. Widchuda Meeim from Thailand Bureau of Quality Control of Livestock Products.

They have each won and will shortly receive a Williams Sonoma BBQ Tools Set! Included in a stainless-steel case for easy storage, these sleek grilling tools are perfect for those upcoming summer cookouts!

Congrats to our quiz winners and happy grilling!

Thank you all for your submissions! 

The correct answer to the Sifting Retention Times – Carbamate Quiz:

Leaking proportioning valve. The leaking proportioning valve improperly mixed the method gradient and didn’t have enough methanol which caused the analytes to elute late.

Chromatography Quiz #27: Only AMPA

What is causing the bad chromatography in the example below?  Simply email your answer as well as your full contact information to Rebecca at rlsmith@pickeringlabs.com by September 1, 2017 in order to win.  You will receive email confirmation that your submission has been received.  The answer to the quiz and winner congratulations will be published in the next issue (to be anonymous, please notify Rebecca in submission). 

Glyphosate Analysis – Only AMPA

Pinnacle or Vector PCX post-column instrument is being used, in a traditional HPLC setup as recommended by Pickering Laboratories. The quiz question: what is causing Glyphosate to disappear?  

Post-column conditions for carbamates analysis:

Reagent 1: GA116
Reagent 2: o-Phthalaldehyde and Thiofluor in GA104
Reactor: 36 °C, 0.5 mL
Reagent flow rate: 0.3 mL/min
Injection volume: 10uL

FLD Settings:

λex 330 nm
λem 465 nm

HPLC Flowrate: 0.4 mL/min
Column Temperature: 55°C


 

Good Chromatogram

Glyphosate Test Mix, 2.5ppm, 10µl Injection

Bad Chromatogram only shows AMPA peak. No Glyphosate peak can be detected.

Glyphosate Test Mix, 2.5ppm, 10µl Injection

 

Pickering Laboratories presents new products at PITTCON 2017

Chicago, McCormick Convention center, March 5-9. Booth # 2625

Pickering Laboratories will be exhibiting at the 4-day event and meeting with customers and distributors to highlight new applications and products from the Product Testing Solutions and Post-Column Derivatization product lines.

New Post-Column Applications:

  • Theanine
  • Glyphosate in Foods
  • Carbamates in Foods
  • Formaldehyde
  • Amino Acids in Pharmacopoeia 8.0

Our Product Testing Solutions include artificial Body fluids manufactured testing made to official industry protocols:

  • Artificial Perspiration
  • Artificial Saliva
  • Artificial Urine
  • Artificial Sebum 
  • Artificial Cerumen

Also we are announcing our new Artificial Sebum and Sweat Emulsion product!

Twice-a-day raffle to win a Fitbit Flex – come to Booth 2625 and get into the game!

 

Glyphosate Banned in France and Labeled a Carcinogen in California

Events surrounding Glyphosate testing in foods continue to evolve with the latest stories “France banning Glyphosate sales in consumer nurseries” and “California requiring labeling Glyphosate as a carcinogen.” We also want to discuss the EU- wide petition to ban Glyphosate.

After an arm of the U.N.’s World Health Organization (WHO) identified the main ingredient in Monsanto’s popular weed killer Roundup as “probably carcinogenic to humans,” France has taken a step to limit sales of the herbicide. http://www.newsweek.com/france-bans-sale-monsantos-roundup-garden-centers-after-un-names-it-probable-343311

A judge tentatively ruled that California can require Monsanto to label its popular weed-killer Roundup as a possible cancer threat despite an insistence from the chemical giant that it poses no risk to people. https://phys.org/news/2017-01-california-monsanto-popular-weed-killer.html#jCp

The European commission says it has received a European Citizens’ Initiative (ECI) – essentially a petition put together by EU citizens – proposing a ban on the controversial pesticide Glyphosate. The proposal is being supported by a number of environmental groups, and according to the rules ECIs need to be submitted by a committee which includes representatives from at least seven EU member states. The initiative calls on the commission ‘to propose to member states a ban on Glyphosate, to reform the pesticide approval procedure, and to set EU-wide mandatory reduction targets for pesticide use’. Several environmental organizations, including Greenpeace and the Pesticide Action Network, have already voiced their support. https://www.chemistryworld.com/news/appeal-to-european-commission-to-ban-glyphosate-gets-go-ahead/2500267.article

Here are links to our earlier posts, if you’d like to catch up on the backstory:

Pickering Laboratories’ Glyphosate testing in foods.

https://www.pickeringlabs.com/library/method-abstracts-2/method-abstract-211/

FDA halted the testing of Glyphosate in food products. No time given for resumption of the testing. 

http://www.foodsafetymagazine.com/news/fda-halts-testing-of-glyphosate-a-possible-carcinogen/

EFSA: Pesticide risk to consumers remains low.

https://www.efsa.europa.eu/en/press/news/161026

The EPA was to hold public meetings Oct. 18-21, 2016 on the safety of Glyphosate. These meetings were postponed over industry objections to the panel members.

https://www.epa.gov/sap/carcinogenic-potential-glyphosate-postponed

The EPA global risk assessment of Glyphosate has been removed from the website. Already two years late, the best estimate now for publication is April 2017 said an EPA spokesperson.

http://www.reuters.com/article/us-usa-glyphosate-epa-idUSKCN0XU01K

The European Food Safety Authority (EFSA) has tested 83,000 food samples for pesticides and reported that most were within safety standards for pesticides residues.

http://www.foodsafetymagazine.com/news/efsa-pesticide-residues-in-food-pose-low-consumer-risk

 

Post-column Method for Analysis of Theanine in Tea

Pickering Laboratories has reported earlier that we developed and validated a post-column method for analysis of Theanine in tea (Camellia sinensis) dietary ingredients and supplements. Theanine is the main naturally occurring amino acid found in tea and it is responsible for a number of health benefits of tea as well as for its savory pleasant taste. 

The analytical method was developed in response to call for methods issued by Stakeholders Panel for Dietary Supplements. The method implements a simple extraction procedure without any clean-up steps and uses cation-exchange chromatography and post-column derivatization with Ninhydrin reagent to separate and detect Theanine.

Pickering method was approved by Expert Review Panel as AOAC First Action Official method for analysis if Theanine and can be implemented by laboratories for analysis if wide range of complex green tea-containing  dietary supplements in forms of powders, tablets, tinctures, gelcaps, sofgels and capsules.

The method and validation results are published in Journal of AOAC International:

J AOAC Int. 2016 Nov 1, 99(6), 1470-1478.

Maria Ofitserova, Sareeta Nerkar

Analysis of Theanine in Tea (Camellia sinensis) Dietary Ingredients and Supplements by High-Performance Liquid Chromatography with Postcolumn Derivatization: Single-Laboratory Validation, First Action 2016.10.

NACRW 2017 Student Scholarships

The deadline is April 21, 2017

We are pleased to announce that NACRW will again be offering five student stipends—where undergraduate and graduate students can apply, and, if chosen, will receive a $500 stipend for travel to the NACRW 2017 conference.

.

If you have any questions, please contact Sareeta Nerkar (organizing committee member for NACRW) at sareetan@pickeringlabs.com.

Information to submit an abstract and register for the workshop are now available online at www.nacrw.org.

  • Advanced detection techniques
  • Advanced sample preparation
  • Novel and Emerging Food Contaminants
  • Veterinary Drugs and Anti-microbial Resistance
  • Residue Analyses in Aquaculture Products
  • Mass Spectrometry Forum: MS applications, challenges 
  • and solutions
  • General Topics
  • Natural Products, Supplements, and Cannabis
  • Updates from USA State/Federal government: agricultural, environmental and health laboratories

For more inforation, please click here.

 

 

A Legacy of Guaranteed Chemistry

By Rebecca Smith, Director of Operations

As most of you have already learned from Jim Murphy in his earlier notifications, our founder and friend Dr. Michael Pickering has passed away.  He is survived by his wife, Judy Pickering, who will now assume ownership of the company.  Michael also leaves behind four children and six grandchildren. 

At the lab, Michael leaves a legacy of another kind.  Pickering Laboratories is a unique place to work, bonded by a strong family feeling and staffed by dedicated employees.  Michael was always the chemist behind the company and from early on he created an unprecedented industry standard: he set out to provide Guaranteed Chemistry. 

Michael started the lab with a background in Amino Acid Analysis and a fantastic improvement on the traditional Ninhydrin reagent.  Our flagship product TRIONE® kicked off the company, but Michael soon expanded into post-column instrumentation kits and other applications.  As his reputation developed as the post-column expert, he began receiving calls from other labs trying to fix different post-column methods.  And Michael loved being challenged by technical problems, so from there our environmental applications were born.  Michael set out to understand the impossibilities with the early EPA methods for Carbamates and Glyphosate, and improve the functionality (and solubility!) of those methods for chemists around the country.  Eventually Michael and his early customers succeeded in updating EPA methods 531 and 547, and a new generation of chemists was grateful (myself included).

When I was originally hired by Pickering Labs, it was as Michael’s research assistant.  And as I try to think of personal anecdotes to share, what I am mostly struck by is that every single person who conversed with Michael has a personal anecdote.  He was a charming and enthusiastic conversationalist.  Michael was both a brilliant chemist and a lover of art, books, food and film.  In any given workday, I would be as likely researching a new sulfonation of a potential reagent as I would be looking up an old Marlon Bando movie (and adding it to my Netflix queue).  We talked about Salvador Dali exhibits he’d seen and about longstanding friendships he cultivated with chemists around the world.  Michael genuinely bonded with everyone he encountered – and I can hazard a guess that if you’d ever had Michael in your lab troubleshooting, I’ve heard about you, your family, your favorite book, what your analytical problem was and how he fixed it.  Michael told great stories, and I hope you had the opportunity to hear one or two from him over the years.

As 2017 marks our 35th year in business, we are striking out on perhaps our most difficult chapter as Michael’s absence will be poignantly felt.  But we hope to heal through our work and honor his legacy by building relationships and solving technical problems for decades to come.  

Please do us the great favor of raising a glass and toasting to a wonderful man.  We celebrate Michael and the years of joy and memories he gave us.

Cheers,
The Pickering Labs Team

 

Chromatography Quiz #26

Chromatography Quiz #25 – B@$eL!nE Noise! — Results

Pickering Labs would like to congratulate the winners of our last newsletter’s Baseline Noise Quiz: Joel Fray from Colorado Analytical Laboratories, Jim Balk from Nebraska DHHS Public Health Environmental Laboratory, Narjes Ghafoori from LA County Environmental Toxicology Lab, Hossein Hajipour from Texas Dept. of Health Services Laboratories, and Tom Schneider from Suffolk County Water Authority.

They have each won and will shortly receive a decadent Chocolate Dream Gift Basket! Created by Cherry Moon Farms, this lovely basket is the ultimate assortment of chocolate sweets that will surely delight! Congrats to our quiz winners and enjoy the goodies!

Thank you all for your submissions! 

The correct answer to the Amino Acids Baseline Noise Quiz:

The zoomed baseline exhibited sine wave with regular oscillations at frequency of about 6 sec. This type of pattern is characteristic to HPLC pump noise as reciprocating HPLC pump moves to deliver the flow of eluants through the column.  If pump is operating normally, the oscillations are very small and will not show as baseline noise. But if the pump has dirty/bad check valves or old/poorly installed seals, the noise increases. In our case, the HPLC pump check valves were bad and needed replacement. 

Chromatography Quiz #26: Shifting Retention Times – Carbamates

What is causing the retention time shift in the chromatogram below?  Simply email your answer as well as your full contact information to Rebecca at rlsmith@pickeringlabs.com by May 1st, 2017 in order to win.  You will receive email confirmation that your submission has been received.  The answer to the quiz and winner congratulations will be published in the next issue (to be anonymous, please notify Rebecca in submission). 

Carbamates Analysis – Shifting Retention Times

Pinnacle PCX post-column instrument is being used, in a traditional HPLC setup as recommended by Pickering Laboratories. The quiz question: what is causing the shifting retention times? 

Post-column conditions for carbamates analysis:

Reagent 1: CB130
Reagent 2: CB910/Thiofluor/OPA
Reactor: 100 °C, 0.5 mL
Reagent flow rate: 0.3 mL/min
Injection volume: 10uL

FLD Settings:

λex 330 nm
λem 465 nm

HPLC Flowrate: 1.0 mL/min
Column Temperature: 42 °C

Good Chromatogram

Bad Chromatogram

 

Guaranteed Chemistry