Analytical Chemistry & Separation Sciences 2020

Solid phase extraction has become a preferable technique for reducing matrix effects for sample preparation due to its ease of use and limited time requirements. MilliporeSigma has launched new  SPE products containing our new SupelTM Swift HLB sorbent.  This hydrophilic-lipophilic balance, HLB sorbent may be used for various compounds over a wide range of polarities and Log P. In this webinar, we will discuss the properties of this sorbent followed by it’s uses in applications involving pharmacological analytes from plasma and also veterinary drugs from bovine milk.

Learning Objectives:

1. Learn about the broad applicability and general methodology of SupelTM Swift HLB for solid phase extraction

2. See application methods and data when using SupelTM Swift HLB for SPE

3. Learn about the many advantages of SupelTM Swift HLB for sample preparation

Starch and flour are important ingredients that determine the quality and carbohydrate nutritional value of human foods, pet foods, and animal feeds. In the agri-food field, there has been a continuous interest in advancing our understanding of the functional characteristics and digestibility of starch and flour under high-temperature cooking conditions (> 100°C). This presentation will cover our recent research of utilizing differential scanning calorimeter, Rapid Visco Analyzer 4800, and texture analyzer to characterize the thermal, pasting and gelling properties and/or in vitro digestibility of different starches, resistant starches, and flours over cooking temperatures of 95-140°C. For commercial isolated starches of different botanical origins, amylose contents and thermal properties are important factors influencing their pasting and gelation behaviors at different heating temperatures. Commercial resistant starches of type 2-4 were cooked at 95-140°C to measure their in vitro digestibility, and the mechanisms of how the digestibility was affected by their thermal, pasting and gelling properties were clearly elucidated. With the gained understanding, functionalities of commercial flours from various botanical sources were also analyzed after cooking over 95-140°C. Different from high-purity starches and resistant starches, it was revealed that chemical compositions and particle sizes of the flours also played a vital role in determining their thermal, pasting and gelation behaviors. The presented new knowledge will be beneficial for the agri-food industry to jointly deploy the aforementioned instruments to evaluate and predict the performance of starch and flour ingredients under high-temperature processing conditions, such as in canning, extrusion and jet-cooking, which thus can be used to maintain and improve the quality and nutritional value of the final products.

Learning Objectives:

1. Understand the functionalities and digestibility of starches at high heating temperatures as measured jointly by DSC, RVA 4800, and texture analyzer

2. Acquire new knowledge on the behaviors of flours at high cooking temperatures as revealed jointly by the three instruments

3. Gain a greater understanding of how different processing and modification methods influence the functional attributes and digestibility of starches and flours

Cannabis is a complex and difficult matrix to work with and the analysis of pesticides in cannabis is a notoriously problematic task. There is major ion suppression present from the significant cannabinoid and non-target analyte concentration. Instrument contamination is another serious consideration in routine analysis and sample cleanup may reduce time between cleanings. Rapid throughput and accuracy are critical in commercial laboratories and instrument downtime can cause major delays in turnaround time and revenue. This presentation will discuss using dispersive solid phase extraction in the analysis of pesticides in cannabis flower and oil as well as strategies for maximizing pesticide sample throughput in a commercial cannabis laboratory.

Learning Objectives:

1. Explain why dSPE can be important for improving pesticide analysis

2. Explain the basics of pesticide analysis in cannabis

3. Identify the importance of good sample preparation prior to analysis

As ‘omics research advances, separations data such as chromatograms and nuclear magnetic resonance (NMR) spectra are being used as direct inputs to machine-learning algorithms ranging from principal components analysis to deep-learning neural networks. Using the data in this way would be improved by an ability to compare data across a wide range of instruments and facilities, but efforts have been hampered by a lack of harmony among measurements. There is, therefore, a need for quality control for the processes producing chromatographic and spectral data, which denotes the need for suitable reference materials (RMs). Presently, certified RMs contain reference data only on their composition or other physical properties. If data processing will involve spectral data, RMs should be certified for spectral profiles, and there is not yet a broadly accepted methodology for doing so. In this talk, I will present the results of recent NIST efforts in harmonizing metabolomic and proteomic measurements using data from interlaboratory studies. These efforts have resulted in a software package, interlab_py, which applies a mathematical procedure for automatically comparing spectra, assigning scores and determining outliers in populations of similar spectra, and identifying facilities which may have consistent process problems. The use of this procedure on data from two interlaboratory studies will be discussed, one using synthetic, biologically relevant metabolite mixtures and one using the NIST monoclonal antibody.

Learning Objectives:

1. Understand the need for reproducible measurements in spectral and chromatographic data

2. Understand the basic principles behind the interlab_py software and its application to interlaboratory comparison of spectral data

Cannabis testing laboratories play a pivotal role in the multidimensional cannabis industry. Production companies to the consumers, whole cannabis community rely on the analytical results produced by the laboratories. Given the immense importance, it is the responsibility of testing laboratories to produce precise, accurate, and consistent results for every sample they analyze. Quality controls including the Quality control (QC) checks, that a laboratory runs in every batch, are determining factors for the certainty of the results. Quality control checks are not only to satisfy the regulatory boards but to have confidence in the results produced. From calibration to the sample runs, every batch should consist of quality control checks. It should be ensured that QC checks such as method blank, technical blank, laboratory control sample, and continuing calibration verifications are passed before analyzing the data for the rest of the samples. Blind testing such as proficiency testing promptly helps in maintaining the accuracy of the instruments and the analysis. When the whole cannabis industry is proceeding towards the standardization, testing laboratories as well are working on it. As of now, a clearer picture for the ultimate standardization of Cannabis testing laboratories is not visible, however, the debate has been started on how it should look like, a plateau, or a peak? I will be presenting on how the quality control in testing laboratories impacts the whole cannabis industry and how a testing laboratory can maintain a good quality control system. I will also be discussing how the future looks like for testing laboratories.

Learning Objectives:

1. Understand how the quality control in testing laboratories impacts the whole cannabis industry and how a testing laboratory can maintain a good quality control system

2. Understand how the future looks like for testing laboratories

Accurate characterization of monoclonal antibodies is essential to development of biotherapeutics. Thorough understanding of biotherapeutic properties aids in the optimization of bioprocess production, product formulation, and product dosage.  This webinar will discuss how to create a complete workflow for monoclonal antibody analysis, including intact analysis, HC and LC subunit analysis, peptide mapping, and N-linked glycans analysis using the advantages and versatility of high-resolution QTOF-MS detection paired with fluorescence detection.

Learning Objectives:

1. Identify the elements of a monoclonal antibody (mAb) characterization workflow

2. Explain the importance of N-linked glycans to the function and quality control of mAb therapeutics

3. Correlate fluorescence and MS data for effective N-linked glycan analysis

Ice formation is a global issue that poses serious challenges for many applications. Certain species in colder regions of the world have adapted to that climate by producing antifreeze (glycol)proteins (AF(G)P) which exhibit ice recrystallization inhibition (IRI). Although several synthetic approaches for the exploitation of these proteins have been investigated, challenges remain in the synthetic design of biomimics. Poly(vinyl alcohol) (PVA) is by contrast a quite simple macromolecular structure and happens to be IRI active, yet many fundamental relationships between structure and performance remain. Here, we were inspired by anti-freeze proteins (AFP), such as the ice-facing right-handed parallel beta-helix in the AFP present in the desert beetle Anatolica polita (ApAFP752) presenting threonines in an ordered array. Drawing comparison between the distance between hydrogen bonding sites in that array, we describe our approach to position small organic molecules with known anti-freeze properties (such as ethylene glycol) pendent to a host polymer chain with consideration of their conformational freedom. We have built systematic variations into both the backbone and side-chain structures and have observed tremendous impact on IRI behavior for several of our polymer scaffolds. FT-IR and NMR were used for confirmation of the functionalized polymer structures, where differential scanning calorimetry (DSC), XRD, and microscopy assays were used to observe the ice IRI behavior. Thermal hysteresis activity (THA), a depression of the freezing point without impact on the melting point (of water, here) is also characterized and corroborated with the IRI trends. The findings in this study will help pave the path for rational design of synthetic AF polymers, useful for applications such as anti-icing coatings through to cryo-preservation methods for organ transport.

Learning Objectives:

1. Define and show application of a variety of analytical performance assays for anti-freeze related behavior for proteins, peptides, and polymers

2. Contrast the performance, via these analytical techniques, of small molecule versus macromolecular performance of similar functionality

3. Understand key structure/property relationships for macromolecule-ice interaction

There are many obstacles to overcome when analyzing Heavy Metals in Cannabis by ICPMS.  Cannabis matrices can be difficult to prepare and analyze due to the complex components of products that occur naturally, as well as ingredients utilized during the manufacturing process.  Often many laboratories have difficulties analyzing cannabis and hemp products due to the variety and variance of complex product matrices.  The Cannabis and Hemp industries are vastly expanding into all spectrums of consumer goods. At Perkin Elmer, we have dedicated an entire team to the study of Cannabis and Hemp including infused products.  Utilizing our NexION ICP-MS, Titan MPS Microwave Digestion System and Standard Operating Procedure (SOP) analyzing Heavy Metals in Cannabis has become simpler.  Sample preparation is one of the biggest hurdles a laboratory can face, as each product and its ingredients present a different obstacle to sample preparation optimization affecting your laboratory’s throughput. We can provide a robust sample preparation guide and supplemental assistance as your lab capabilities expand and projects diversify.  A proper digestion protocol and a robust ICPMS analytical method are critical to your laboratory’s success. PerkinElmer’s NexION ICPMS utilizes Universal Cell Technology (UCT) to aid in the removal of polyatomic interferences for accurate and reliable analytical data. Please join us to discuss how our instrumentation offerings and validated analytical methods can help your laboratory be on the cutting edge of Cannabis Testing for Heavy Metals.

Learning Objectives:

1. Identify possible sources of interferences and analytical challenges found during analysis  of Heavy Metal contamination in Cannabis  and Cannabis derivatives by ICPMS

2. Understand typical sample preparation techniques for Cannabis and Cannabis derivatives utilizing closed-vessel microwave digestion

Pesticides are routinely applied to crops to prevent or control pests and are therefore routinely tested for the presence of pesticide residues and to check for compliance with permitted Maximum Residue Levels (MRLs).  Given the globalization of the food supply, the large number of pesticides used, and the number of samples to be analyzed, robust, accurate, reproducible, and cost-effective multiresidue methods are the preferred to maximize screening capabilities per sample.  Liquid chromatography coupled to mass spectrometry (LC-MS) is the preferred method for performing multiresidue analysis due to the ability to screen and accurately measure 100’s of pesticides at or below MRLs with high confidence.  Targeted analysis using selected reaction monitoring (SRM) on triple quadrupole mass spectrometers is the most common approach as state-of-the-art triple quadrupole mass spectrometers can successfully monitor over 500 compounds in a 15-minute experiment.  SRM methods require the analyst to set up the instrument to screen for specified compounds requiring a priori knowledge of precursor/product ion m/z values as well as expected product ion ratios for confirmation. Recently, untargeted workflows have been developed based on high resolution/accurate mass (HRAM) analysis that does not require pre-defined compound lists.  HRAM MSn analysis enables analysts to detect and characterize known pesticides as well as unknown compounds that may be associated with unregistered pesticides or breakdown products.  Detection of such compounds can then be further verified and added to known pesticide lists through development of new standards. These two methods work in harmony to provide the most comprehensive workflow to address pesticide screening and enhance food safety.  The presentation will cover each workflow from common sample preparation to the different data acquisition methods and automated data processing.

Learning Objectives:

1. Identify intelligent untargeted data acquisition routines

2. Define empirical data metrics used to confidently annotate unknown molecules

3. Explain current approaches to integrate results from untargeted sample analysis to targeted SRM panels for high-throughput screening/quantitation

Food safety is arguably the most important segment of food science and analysis.  From residual pesticide contamination to allergens to mycotoxins, there are many ways food can be harmful to human health.  Food producers and processors, as well as independent testing labs conduct rigorous testing that can be verified and objectively recorded.  To get accurate and reproduceable results that are legally defensible in court, these labs rely on analytical instrumentation as the centerpiece of their efforts to ensure a safe food supply. In this presentation we will provide a brief introduction to food safety testing, and then describe how state-of-the-art analytical instrumentation is used in the food safety industry.  Specific examples will include GCMS and LCMS for residual pesticide at trace levels and mycotoxins, ICP-MS for heavy metals, and MALDI-TOF for pathogens like salmonella.  Additionally, we will discuss the contribution of food packaging and food contact materials (FCM) to food contamination.

Learning Objectives:

1. Understand the challenges in food testing

2. Illustrate current approaches to food safety testing

3. Demonstrate the power of analytical instrumentation in food safety testing