Analytical Chemistry & Separation Sciences 2020

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

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

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

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