Patrick Lavery is an Editor for the MJH Life Sciences brands LCGC and Spectroscopy, and their respective websites, 

. He previously spent nearly a decade as a news anchor, reporter, and producer at New Jersey 101.5 FM.

Patrick Lavery

The rising popularity of diclofenac sodium spheres as a drug delivery system is the subject of a new study in 

Spectrochimica Acta Part A: Molecular and Biomolecular Spectroscopy

 that examines the drug loading of diclofenac sodium and release rate during the coating process (1). Not only were drug loading and release rate monitored, but both were given real-time, in-line predictions with the use of near-infrared (NIR) spectroscopy.

diclofenac word display on tablet | Image Credit: © JoyImage - stock.adobe.com

The 13-author study was a collaboration between researchers affiliated with Shandong University and Shandong SMA Pharmatech Co., both in Shandong, China. They began their report by explaining how process analytical technology (PAT) has been increasingly incorporated into manufacturing best practices in the pharmaceutical industry in recent years, with PAT being described as an indispensable and powerful tool for the in-line and real-time control and monitoring of drug production, whether with NIR, Raman spectroscopy, or optical coherence tomography (OCT) (1).

Diclofenac sodium enteric-coated tablets are commonly prescribed in the United States under the brand name Voltaren, which is also offered in gel form (2,3). It is a nonsteroidal anti-inflammatory drug (NSAID) that is used for arthritis relief, providing anti-inflammatory, analgesic, and antipyretic effects according to the U.S. Food and Drug Administration (FDA). The research team in Shandong, meanwhile, reported that diclofenac sodium spheres, as a multi-unit, film-coated drug delivery system, offer good fluidity and a stable release rate, with fluidized bed coating widely used in industrial production (1).

Fluidized bed coating involves the spraying of a functional polymer with coating dispersion, generally leaving a uniform film coating. It has the advantages of fast heat and mass transfer, a large contact area between gas and solid phases, and a small temperature gradient (1). As part of this process, the researchers said, testing and analysis of the drug loading and release rate—the critical quality attributes (CQAs) of diclofenac sodium—ensures the delivery system’s safety and efficacy, but off-line methods are time-consuming in such a way that delays analysis unnecessarily.

In this application, a real-time in-line prediction model using NIR spectroscopy allowed for strong anti-interference, in turn permitting sucrose spheres to be introduced into the experiment in varying feeding amounts (1). The researchers said such a design would prove the robustness of the model.

Near-infrared spectroscopy is used where multicomponent molecular vibrational analysis is required in the presence of interfering substances. The near-infrared spectra consist of overtones and combination bands of the fundamental molecular absorptions found in the mid-infrared region. Near-infrared spectra consist of generally overlapping vibrational bands that are non-specific and poorly resolved. The use of chemometric mathematical data processing can be used to calibrate for qualitative of quantitative analysis despite these apparent spectroscopic limitations.

A micro NIR spectrometer with a diffuse reflection module and high-temperature external probe was used in concert with the procedure of fluidized bed coating. Results of this experiment were said to be successful, with the team finding it was able to verify the analytical ability of the model. Because of this, the authors suggested further study would be done in this area, to give more scientific backing to intelligent and modern drug manufacturing processes.

(1) Sun, Z.; Zhang, K.; Lin, B.; et al. Real-Time In-Line Prediction of Drug Loading and Release Rate in the Coating Process of Diclofenac Sodium Spheres Based on Near Infrared Spectroscopy. 

(2) Voltaren® (diclofenac sodium enteric-coated tablets) – Tablets of 75 mg – Rx only – Prescribing Information. 

https://www.accessdata.fda.gov/drugsatfda_docs/label/2009/019201s038lbl.pdf

Voltaren Arthritis Pain Relief Gel & Dietary Supplements | Voltaren

Articles

The method of analysis described by these researchers had the advantages of being in-line and in real time, compared to more traditional approaches such as high performance liquid chromatography (HPLC).

Near-Infrared Spectroscopy Predicts Drug Loading and Release Rate of Coating of Diclofenac Sodium Spheres

Researchers in Germany, some of whom are associated with the Rathgen Research Laboratory (Rathgen-Forschungslabor der Staatlichen Museen) in Berlin, recently published a report on work done by that laboratory in 2019 to trace the history of two amber disc beads which were first discovered potentially more than a century earlier, in 1914 (1). The beads, the researchers said, came from a cushion under the large ziggurat, an ancient pyramidal stepped tower, of Aššur, Iraq. Although much of the recent study is historically focused, spectroscopic techniques that were applied to zero in on the beads’ place and time of origin are also described.

Ashur (Qal'at Sherqat), Assyria Historical city, Ninawah Iraq، it was a major ancient Mesopotamian civilization which existed as a city-state from the 21st century BC to the 14th century BC | Image Credit: © humam - stock.adobe.com

Amber's value in ancient time periods stemmed from its captivating appearance and rarity, making it a prized material for ornamental jewelry. Its use as a trade commodity extended its influence across many regions and cultures, while its ability to preserve ancient inclusions added to its beauty as a window into the past. In ancient societies, wearing amber denoted status and cultural significance, underlining its multifaceted appeal.

Specifically, this research team used Fourier transform infrared (FT-IR) spectroscopy, 

which is considered a preferred technique

 for infrared measurements. In the application of infrared (IR) radiation to a given sample, some radiation is absorbed while some is transmitted (passes through the sample). FT-IR measurements provide high resolution infrared spectra, which reveal the detailed chemical composition of samples.

By exposing the amber beads to a broad range of infrared wavelengths, FT-IR spectroscopy enables the identification of specific chemical bonds present within the beads' molecular structure. This non-destructive technique provides valuable information about the composition of amber beads, including the identification of functional groups such as hydroxyls and carbonyls.

In this case, the German team examined fragments of the amber beads with FT-IR, finding that their spectra largely aligned with that of Baltic amber, also known as succinite (1). This was determined despite what the researchers categorized as “heavy weathering,” a natural occurrence given the beads’ initial discovery in a foundation deposit of the ziggurat that is believed to date back to c. 1800–1750 BC. Addressing the historical aspect of their research, the authors hypothesized that the amber may have come to the Middle East in that era as gifts from “well-travelled persons from central or western Europe,” but could have also signaled the future amber trade industry in the Middle East and Mediterranean several centuries later.

Natural amber. Two extraordinarily beautiful pieces of transparent yellow amber with inclusions on a white background with a bokeh effect. A natural mineral for jewelry. Color texture of sunstone | Image Credit: © IGOR - stock.adobe.com

But what might that history mean in the context of any discoveries and knowledge gleaned from prior, modern studies? In spectroscopic analysis of amber, the researchers said, there exists a broad horizontal plane that is characteristic of well-preserved samples; this is known as the “Baltic shoulder” (1). A single C-O band (related to the presence of ester groups [C-O-C=O]) in the spectrum at approximately 1150 cm

 is the most telling feature, with the Baltic shoulder preceding it from roughly 1250 to 1175 cm

 (1). Comparing their sample to previous identifications of Baltic succinite, the researchers said with confidence there was a high likelihood that the amber found in Aššur was of this type, and therefore most likely originated in either the Baltic or North Sea regions.

Baltic sea seascape at sunset, Poland, wooden breakwater and waves | Image Credit: © tomeyk - stock.adobe.com

Although humbly referred here to as “circumstantial evidence,” the likely identification of Baltic amber or succinite in Aššur, Iraq by FT-IR spectroscopy shows how analytical science can play a role not only in future trends, but also in looking back through history and better understanding ancient worlds. The research team that put forth this study said their discovery makes it possible to imagine that as far back as the early 2nd millennium BC, people traveled with valuable cargo from central Europe to possibly Mesopotamia, indicating nascent attempts at globalization and commerce in this early period.

(1) Bunnefeld, J.-H.; Becker, J.; Martin, L.; Pausewein, R.-R.; Simon, S.; Meller, H. Baltic Amber in Aššur. Forms and Significance of Amber Exchange between Europe and the Middle East, c. 2000–1300 BC. 

Fragments of amber beads examined in 2019 showed a Fourier transform infrared (FT-IR) spectrum consistent with Baltic amber, or succinite, suggesting the artifacts came from the Baltic or North Sea regions.

FT-IR as a Determinant of Age and Origin Location of Baltic Amber Beads in Aššur, Iraq

 has documented the use of spectroscopy and related techniques to explore the origins of human-made wooden tools from the Middle Pleistocene era, specifically a double-pointed "throwing" or hunting stick (1). According to the study's authors, the area that is now Schöningen, Germany, where these tools were first discovered in 1994, is home to the oldest large-scale record of such hunting equipment.

 asked Annemieke Milks, a British Academy postdoctoral researcher in the department of archaeology at the University of Reading, UK, and Dirk Leder of the Lower Saxony State Office for Cultural Heritage in Hannover, Germany, two of the co-authors, about their research in terms of spectroscopy's place in determining the construction of these tools and therefore, the level of sophistication in woodworking skill of these early humans about which there is still much modern uncertainty.

Double-pointed wooden throwing stick: perspective image | Image Credit: © Volker Minkus - CC BY 4.0

As your text states, the Schöningen site was discovered nearly 30 years ago, but many questions remain. You say that this double-pointed stick was carved from spruce, but in other ways it differs from other wooden tools found. How so?

 There are several aspects that unite the wooden weapons from the ‘Spear Horizon’, the specific area and time period from which the spears and throwing sticks were found. Like this throwing stick, the spears were crafted to be double-pointed. What makes the throwing stick different in design is that it is shorter than the spears. It was also shaped from a smaller, naturally curving branch, to reflect a finished shape that was curved rather than straight. These features, in addition to the specific way that the stick was shaped to have a slightly elliptical cross-section, all point to intentional design as a projectile weapon, thrown rotationally like a boomerang. In contrast, the spears look like were designed to be both thrust and thrown overhand like javelins.

Composite image of the micro-CT slices at regular intervals, illustrating the change in diameter and shaping strategy. | © Photo: V. Minkus. micro-CT scans: Waygate Technologies and T. Koddenberg. Illustration: A. Milks - CC BY 4.0. DOI: 

Overview photo of the double-pointed stick. | Image Credit: © Volker Minkus - CC BY 4.0. DOI: 

How much is generally known about life in the Middle Pleistocene era and what clues do these tools hold?

 Unfortunately, we still know relatively little about the time before Neanderthals, so more than 300,000 years ago. People lived as hunter-gatherers roaming the landscape in extended families and bands. They ate both plants and meat, and lived under the open sky, probably in tents, rather than in caves. When thinking about this early part of the Stone Age most people would associate it with handaxes, but at Schöningen, it seems that the stone tools used were limited to simple stone flakes. This stands in contrast to their range of different wooden weapons, shaped with sophisticated woodworking skills. The Middle Pleistocene may also be the time when hominins started caring for their deceased and might have had an aptitude for symbolic expressions, although this is much debated and evidence remains sparse.

It’s fascinating that spectroscopic techniques can not only analyze a tool of this sort to evaluate human behavior regarding its construction and use, but also the types of animals it might have been used to hunt. What other information can spectroscopy provide?

 Spectroscopy has the advantage over other methods that it is non-destructive or at least minimally invasive, which is an important benchmark in archaeology as we are responsible for objects that are both ancient and often unique.

Spectroscopy provides a great range of opportunities for analyzing chemical elements, minerals, and biological residues, which provide us clues on the materials used, for example in cave or pottery paintings, blood and plant residues on stone-tipped weapons or metal vessels, components of adhesive materials or metal alloys. For example, gold applications on the sky disc from Nebra in Germany could be linked to geological sources in Cornwall, UK, while copper of the bronze alloy was imported from Austria speaking for a vast trading network spanning Europe some 4,000 years ago.

Are there other periods of prehistory you can think of that contain the level of mystery uncovered by the finding of these tools, and what might future deployment of the techniques used here tell us about our predecessors?

 Every period in archaeology has its own research agenda, however generally speaking, raw material sources and material components are a fast-growing field of interest in archaeology. Alongside better understanding of raw material sources and material composition stand questions of prehistoric technologies and the level of skill reached by the craftspeople of their time. Personally, I believe spectroscopic methods will play a crucial role in better understanding our past.

Excavation photograph of the double-pointed stick. | Image Credit: © Peter Pfarr - CC BY 4.0. DOI: 

Any other points you would like to make about this research or how you might continue it in the future?

 At Schöningen we are currently studying the complete assemblage of wooden tools from the so-called spear horizon, while in future there might be opportunities to also study even older tools from different zones at Schöningen. As for spectroscopy analyses, we intend to broaden our investigation of residues on wooden hunting weapons. We are looking for clues of blood, grease or plant remains on the tips of spears.

(1) Milks, A.; Lehmann, J.; Leder, D.; et al. A double-pointed wooden throwing stick from Schöningen, Germany: Results and new insights from a multianalytical study. 

Editor Patrick Lavery of Spectroscopy talked to two co-authors of a study that analyzed information about a 300,000-year-old wooden hunting stick found in modern-day Germany.

Spectroscopic Techniques Reveal Sophistication in Hunting Tools of Middle Pleistocene Humans

Spectrochimica Acta Part B: Atomic Spectroscopy

 measures the optimization potential of the increasingly popular atmospheric pressure plasma jet (APPJ) by using optical emission spectroscopy (OES) to determine certain parameters such as plasma temperature (T

) (1). The authors said OES has the capability to analyze up to 17 emission lines of neutral and singly-ionized argon species, respectively Ar (I) and Ar (II)—as APPJs function by running an electric discharge under argon gas flow—but stark differences in the intensities between Ar (I) and Ar (II) expose some fundamental limitations to this mode of spectroscopy, which a methodology newly developed in this study aims to resolve.

Close up of the Argon symbol in the periodic table, tech space environment. | Image Credit: © Tom - stock.adobe.com

The researchers, hailing mainly from the Institute of Applied Physics at Johannes Kepler University in Linz, Austria, said APPJs have attracted interest mainly in the last decade in various fields of study, from coating applications to biomedical uses to surface technology including cleaning and surface modification (1). Their ease of use and ability to be deployed in ambient air make APPJs particularly well-suited to industrial use, in the authors’ opinion, but to fully understand these devices’ capabilities, plasma characteristics must be measured. Such characteristics encompass not only T

, but also adjustable properties such as the electric power of the plasma generator, gas flow, and distance from the exit via the jet nozzle.

Optical emission spectroscopy (OES) is recognized as a useful tool in plasma characterization because it is non-invasive and is able to identify species by their distinct spectral signatures, but can be limited by relatively low intensities of ionic emission lines. Accordingly, further explaining the distinction between Ar (I) and Ar (II), the researchers said that Ar (I) lines, which are described as very intense, are well separated, spectrally speaking, from the very weak Ar (II) lines (1).

To attempt to remedy this, the methodology devised for this study used spectral bandpass filters for collection and to amplify the Ar (II) signal-to-noise (S/N) and signal-to-background (S/B) ratios—additionally allowing for accurate calculation of T

 in the APPJ plasma using a Saha-Boltzmann plot (SBP). SBP increases the accuracy of a Boltzmann plot (BP), which has been used in previous studies with OES to determine temperatures of electric discharge and laser-induced plasma. For measurements in the few kW power regime as desired here, the research team opted for SBP analysis instead of BP.

Results garnered in this experiment were described by the researchers as consistent and accurate (1). Typical values of T

. This, the authors said, was in contrast to the inaccuracies and inconsistencies present in plasma characterization using only Ar (I) lines instead of both Ar (I) and Ar (II). In closing, the researchers expressed hope that their study would influence OES of other gas plasma using their novel methodology.

(1) Giannakaris, N.; Gürtler, G.; Stehrer, T.; Mair, M.; Pedarnig, J.D. Optical emission spectroscopy of an industrial thermal atmospheric pressure plasma jet: Parametric study of electron temperature. 

Researchers say the developed methodology, which reconciles the different intensities of neutral and singly-ionized argon species, may be further refined and applied to optical emission spectroscopy (OES) of other rare gas plasma.

Overcoming OES Limitations with New Methodology to Determine Parameters of an Atmospheric Pressure Plasma Jet

’s curiosity with its suggestion that Raman spectroscopy would be a viable approach for the detection of biomolecules, and particularly subsurface biosignatures, on missions to Mars (1). This study paved the way for current Raman studies taking place on the Red Planet (2). Published in the journal 

, the report is the collaborative work of some 37 authors, led by Mickael Baqué and Jean-Pierre P. de Vera of the Microgravity User Support Center at the German Aerospace Center in Köln, Germany.

Astronaut on mars the red planet. Landscape with desert and mountains, Colonization of Mars, generative ai | Image Credit: © viperagp - stock.adobe.com

, de Vera discussed the study and its place within the European Space Agency (ESA)’s BIOMEX (BIOlogy and Mars EXperiment) project, as well as other programs such as ESA’s ExoMars and National Aeronautics and Space Administration (NASA)’s Mars 2020 mission, launched from Cape Canaveral, Florida, USA. He said selected biomolecules showed promise of being picked up by Raman instruments on these or other future rovers, “Some chosen biomolecules and particularly some pigments are resistant to the conditions in space and detectable by Raman spectroscopy if embedded in Mars-like regolith/mineral mixtures in a Mars-like atmosphere and Mars-like surface irradiation,” de Vera said.

How the research team arrived at that conclusion was as part of the near-700-day BIOMEX mission from July 2014 to June 2016, during which four experiments testing the feasibility of Raman spectroscopy were conducted outside the International Space Station (ISS) for a period of 469 days (1). In preparation, seven biomolecules – β-carotene, cellulous, chitin, chlorophyllin, melanin, naringenin, and quercetin–were mixed with two Martian regolith analogs. According to the study, while a regolith surrounding a potential molecule may offer protection and stabilization, it may increase the Raman signal background level, which decreases signal-to-noise ratio (S/N) and accordingly, chances of detection.

The group of biomolecules was first exposed to simulated Mars conditions in low Earth orbit (LEO), as amino acids and DNA had been in previous analysis–although not by Raman spectroscopy (1). But the researchers said that critical factors of the Martian environment, including photonic and ionic radiation, could not be simulated with high fidelity on Earth, leading to the four experiments on ESA’s EXPOSE-R2 platform.

Looking back at this process, de Vera explained his team’s hypothesis, “With the main goal to search for extinct or extant life on Mars, the selected biomolecules within the BIOMEX project are resistant to Mars-like conditions and particularly to Mars near-surface and subsurface conditions and could be detectable by the chosen Raman instruments on the rovers,” he said.

UV radiation, along with ionizing radiation and oxidizing compounds, has potential to destroy detectable traces of biosignatures anywhere from the upper centimeters to meters above the Martian surface, according to the researchers (1). But this study found that while UV radiation changed Raman spectra signals strongly, only minor changes occurred when samples were exposed to a UV-shielded subsurface.

The authors suggested expanding the range of biomolecules tested in future exploration, and further recommended implementing a systemic Raman signature database, “Therefore, if life originated and started and evolved on Mars during its habitable phase in its planetary history, Raman spectroscopy is an excellent tool to detect some remnants or complete remaining biomolecules in the near subsurface of Mars,” de Vera said.

The researchers suggested expanding the range of biomolecules tested and emphasized the potential of Raman spectroscopy as a valuable tool for detecting remnants of biomolecules in the near subsurface of Mars. This work has been invaluable for providing insight into the possibility of using Raman spectroscopy to search for past or present organic life on the planet. With such insight, Raman is currently being used to search for biomolecules on the Martian surface (2).

(1) Baqué, M.; Backhaus, T.; de Vera, J.-P.P.; et al. Biosignature stability in space enables their use for life detection on Mars. 

(2) Sharma, S.; Roppel, R. D.; Murphy, A. E.; et al. Diverse organic-mineral associations in Jezero crater, Mars. 

https://doi.org/10.1038/s41586-023-06143-z

Author Jean-Pierre P. de Vera talks to Spectroscopy magazine about his study in which seven biomolecules were exposed to a simulated Martian environment outside the International Space Station (ISS) for a period of approximately 15 months.

Life on Mars? Raman Spectroscopy Tests Stability of Biomolecules at Surface Conditions

Caroline Hroncich, Associate Editorial Director, LCGC / Spectroscopy

Tell us where you’re from, and a little about your background.

 I’m from New Jersey, I grew up in Bergen County and now I live in Hudson County, not too far from the MJH offices. I’ve been working in media for nearly a decade. I’ve written and edited for several consumer and trade publications including Reuters, Business Insider, MarketWatch, CannabisWire, and more. I have degrees from Villanova University and Columbia University.

You're actually returning to the MJH family, correct? What did you do in your previous time here?

magazines, which are both MJH brands. I was an associate editor on the team, and I managed both daily news content and more long-form print pieces. Working at 

got me really excited about science journalism and it’s one of the reasons I’ve decided to come back.

What drew you to this position, and were you familiar with our publications previously?

 are incredibly well-respected publications in their industries. I’ve always been a fan of the work that you are doing and I’m glad that I now get to be a part of it. 

are on the cutting edge of the science and the topics we are covering will have impacts in research for years to come.

Even in your short time on the job, what have you learned about separation science? Did you do a lot of background research before starting here, and what challenges do you expect?

 I am still learning about separation science but as a journalist, I see it as a new and interesting challenge. I’m a very curious person and I’m not afraid to ask questions. Right now, my goal is to meet with as many industry experts as possible to understand their work and how we can continue to cover the topics they are interested in.

In addition to being legacy print brands, LCGC and Spectroscopy also have websites and social media footprints. As we know, people continue to get news and information on their devices more and more every day. Talk about how you envision the continued integration of our print and online products and what readers can expect to see on both sides of that equation.

 I think it is all about balance. We have an incredibly loyal readership, and we’ll continue to publish informative news and peer-reviewed content in print and online. I want our readers to be able to engage with us wherever they are – whether that’s on LinkedIn, by reading the magazine, or at a conference.

What’s it been like meeting and working with our team so far? What are the strengths that you see and how are you planning to use your experience to mold our product?

 We have a great team at MJH. Even in my short time here, I’ve been impressed with how innately curious and passionate everyone is about the topics they cover. We have a team with a variety of talents, and I plan on tapping into that to make our content even better.

Enough about work. Tell us more about yourself. What are your interests, hobbies, fun facts, anything else you’d like to share?

 I spend a lot of my free time with my friends and family. I enjoy cooking, reading, and traveling. I’m a very creative person. I like to paint and have recently gotten into ceramics. I also have two cats that I recently adopted and I’m always sharing photos of them on Twitter (

Anything else you’d like our readers to know as we introduce you to them?

 Just that I’m very excited to be working with our staff editors and the editorial board. I am always available to chat and you can reach out to me at 

LCGC and Spectroscopy magazines recently welcomed Caroline Hroncich to lead their joint editorial staff in print and online. In this interview, Hroncich talks with editor Patrick Lavery about her experience and what readers can expect for the future.