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CHAPTER 9:
IMPORTANCE
OF ANALYTICAL
CHEMISTRY
By: Dr Nadirul Hasraf bin Mat Nayan
OUTLINE
9.1 THE ROLE OF ANALYTICAL CHEMISTRY IN THE DEVELOPMENT OF
MODERN BIOTECHNOLOGY INDUSTRY
▪ Biotechnology has been defined as use of living systems and organisms to develop products and
processes for the benefit of mankind in terms of improved agricultural yields, food production,
medicines and cleaner industrial manufacturing processes.
▪ Over the years, biotechnology has diversified into several branches such as Genetic
Engineering, Industrial Biotechnology, Environmental Biotechnology, Molecular biology,
Genomics, etc.
▪ Meanwhile, analytical chemistry methods refer to techniques used for the detection,
identification, characterization and quantification of chemical compounds. These methods are
commonly used in biology for research, development and quality control of pharmaceutical
products.
9.1 THE ROLE OF ANALYTICAL CHEMISTRY IN BIOTECHNOLOGY
▪The methods used allow quantitative or qualitative, more or less invasive and destructive
analysis of samples, and typically require sophisticated instrumentation.
▪ Along with the knowledge of application of the analytical technique, the researcher also should have the
knowledge of the sampling techniques for the analytical instruments as it is one of the deciding factors to
choose a specific technique for the analysis.
▪ The results obtained by using the analytical equipment are relatively authentic and accurate.
▪ With the development of biotechnology, the usage of analytical equipment has increased by many folds.
▪ The areas of biotechnology such as nanotechnology, cancer biology, genetic engineering and many more are
dependent on the analytical equipment for most of their experimental analysis.
▪ Analytical equipment find its application not only in the research works but also at the industry level.
▪ Various food and pharmaceutical industries rely upon the analytical techniques like FT-IR and Raman for the
quality analysis of the products.
9.1 THE ROLE OF ANALYTICAL CHEMISTRY IN BIOTECHNOLOGY
▪ The most ancient, popular and highly used analytical equipment are
Raman spectroscopy, Infra Red spectroscopy, Gas chromatography
and NMR
9.1 THE ROLE OF ANALYTICAL CHEMISTRY IN BIOTECHNOLOGY
Raman spectroscopy:
FTIR: Fourier transform infra red spectroscopy:
The Raman spectroscopy is derived from an inelastic light
scattering process in which a monochromatic beam of light It is used to identify the functional groups in
usually a Laser photon is directed towards the sample a molecule and can be applied in quality
molecule and it is being scattered after interacting with the control of various pharmaceutical and food
sample molecules. products to compare the purity of a product
with the database collection of pure
compounds. Infra red technique can be
Infra red spectroscopy: applied for the detection of protein by a
process which can be fast and
The spectroscopy which operates in the infra-red region of the
non-destructive.
electromagnetic spectrum is called as infra red spectroscopy. The infra red
region of light has a lower frequency and longer wavelength than visible
light. This technique can be used to identify and study chemicals. Fourier
transform infrared spectrometer is one of the common instruments using
this technique.
9.1 THE ROLE OF ANALYTICAL CHEMISTRY IN BIOTECHNOLOGY
1) Pharmaceutical
• Analytical chemistry underpins pharmaceutical drug development by providing assurance of the quality,
safety and efficacy of new medicines through:
Providing knowledge of compound separation, identification and quantification that can be useful for
measuring bioavailability of drugs, purifying drugs during synthesis, and identifying drug metabolic
pathways.
Accurately quantify drugs and metabolites in pharmacokinetic, transport, and delivery studies, a strong
understanding of analytical chemistry principles is necessary and only well-characterized analytical
methods should be used to ensure the integrity of collected data.
• Quantitative methods used to measure the concentrations of target analytes in biological specimens
should be thoroughly characterized for accuracy and limits of quantification.
• Method characterization requires the use of appropriate calibrators and quality control samples. These
materials should be made in large batches and characterization should be performed for each batch and
any time a new batch of materials is made.
9.2 HEALTH AND WELFARE - PHARMACEUTICAL
❑ Calibration curves should then be analyzed over the course of at least seven runs spanning multiple
days and the accuracy, precision, and coefficient of determination should be calculated for the specific
batch of calibrators.
❑ The choice of calibrator concentrations is extremely important and should not only focus on
sensitivity at the low-concentration end of the calibration curve but should also encompass
reasonable concentrations that would be expected when analyzing unknown samples.
9.2 HEALTH AND WELFARE - PHARMACEUTICAL
2) Medical
• In the field of medicine, analytical chemists help physicians diagnose diseases through
clinical chemistry — analyzing blood gases, enzymes, bacteria, and other medical
samples. Through pathology, analytical chemistry helps us understand disease through
its molecular makeup.
9.2 HEALTH AND WELFARE - MEDICAL
• The use of instrumentation, statistics, chemistry, and computers makes analytical chemists
essential to medical research and pharmaceutical development. And, without analytical
chemistry, there would be no forensic science, the sciences used for the purposes of law.
Analytical chemistry is used throughout the medical device development pathway. This includes the
discovery process, prototyping, preclinical and clinical testing, regulatory decisions, product launch, and
post-market monitoring. Analytical testing is often found in the prototyping and testing stages, which
incorporate feedback loops to redesign new biotechnology.
• In the early phases of discovery + ideation and invention + prototyping, there is an emphasis on
the use of analytical techniques to characterize novel inventions.
• This necessitates chemical imaging techniques such as confocal Raman and surface chemistry
analysis for materials and coatings using techniques like scanning electron microscopy (SEM),
Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), and
time-of-flight–secondary ion mass spectrometry (ToF-SIMS)
SEM XPS
FTIR
9.2 HEALTH AND WELFARE - MEDICAL
•In the preclinical stage, analytical chemistry is especially key to the success of new medical device
technology because it is used for measuring performance and safety characteristics of medical
devices ranging from a material sample (coupon) to a complete device.
•There are thousands of medical devices with different technologies and uses, so performance can
range widely depending on factors such as the indication for use and the anatomic location.
•Testing can include purely nonbiological factors such as adhesion, swelling, or drug elution from a
coating as well as bioanalytical methods such as measuring antimicrobial performance
9.2 HEALTH AND WELFARE - MEDICAL
•Analytical testing is also key for ensuring safety in the post-market process,
for routine lot release measurements, and for investigations of adverse
events and adulteration and contaminants in the supply chain
9.3
ANALYTICAL CHEMISTRY IN
MALAYSIA
ANALYTICAL CHEMISTRY IN MALAYSIA - INTRODUCTION
❖ Much of our daily life is dependent on chemical analysis. Accurate quality-control analysis
ensures the quality of the food we eat, the medicine we use, the water we drink, and the air
we breathe.
❖ Among the sciences, analytical chemistry stands out as a practically versatile, useful and
important field.
❖ Analytical chemistry is comprised of qualitative and quantitative analysis.
Qualitative analysis deals with finding out which substances are in analytical sample
and quantitative analysis determines how much of each substance is in the sample.
❖ Analytical chemistry analysis has many applications in industry, medicine, biochemistry,
physiology, geology, oceanography, and environmental science.
❖ In addition, analytical chemistry teaches special skills and techniques which have relevance
for physicians, engineers, and many other professionals.
ANALYTICAL CHEMISTRY IN MALAYSIA - INTRODUCTION
• All the analytical technique had been applied and published on various of
journal scope to obtain the desired data.
• In the example below, you can see, learn and identify the
techniques/method of analytical chemistry that they used in different area
of field.
ANALYTICAL CHEMISTRY IN MALAYSIA – JOURNAL 1
1) ASSESSMENT OF HEAVY METAL CONTAMINATION IN SQUID (LOLIGO SPP.) TISSUES OF
KEDAH-PERLIS WATERS, MALAYSIA
Introduction
• Nowadays, seafood especially squid (Loligo Spp.) from the Cephalopoda class has a high demand due to their
nutritional values.
• Squids have good-tasting flesh and that makes them commercially favourable among people since the early
80’s.
• Apart from that, they play an important role in the marine ecosystem as they become prey to some marine
mammals.
• However, humans are also indirectly more susceptible to heavy metal poisoning by consuming this organism.
• According to journalist, this species is said to be vulnerable to heavy metal contaminants because of their
feeding habits.
• Contamination from heavy metals may occur due to the marine environment being continuously polluted by
human activities.
• Heavy metals may then transfer to and accumulate in marine organisms through the food chain.
• In this study, copper (Cu), cadmium (Cd), lead (Pb) and zinc (Zn) have become the main focus due to the fact
that all of these elements are found accumulated excessively in squids.
Analytical analysis #only for reading purposes
• In this study, the digestion and analytical procedures were adopted and applied from the Milestone
Microwave Digestion Method (DG-FO-17).
• For this analysis, 0.5 g of the homogenized squid sample was weighed and put into the Teflon vessel. After
that, 7 ml of HNO3 (65%) and 1 ml of H2O2 (30%) were added into the Teflon vessel using a single channel
pipette, 100-1000 microlitre (μl) of the brand CappAero which was ISO 9001; 2000 certified.
• Afterwards, the Teflon bombs were placed into the oven at 200˚C for 30 minutes. The samples were then
poured into centrifuge tubes and filled-up to 10 ml with Mili-Q water. These procedures were later repeated
for the DORM3 (Fish Protein Certified Reference Material for Trace Metals).
• The analysis of Heavy metals concentration was then carried out by using Inductively Coupled
Plasma Mass Spectrometer (ICP-MS) (Perkin Elmer model Nexion 300X).
• For method validation purpose, a certified reference material for trace metals, DORM-3 (Fish Protein
Certified Reference Material for Trace Metals) was digested and heavy metal levels were determined in the
same manner as our samples.
• The limit of detection for each heavy metal was calculated from three standard deviations of eight method
blanks.
Further reading: Jamil, T., Lias, K., Norsila, D., & Syafinaz, N. S. (2014). Assessment of heavy metal contamination in squid (Loligo
spp.) tissues of Kedah-Perlis waters, Malaysia. Malaysian Journal of Analytical Sciences, 18(1), 195-203.
Result analysis
• The accumulations of heavy metals are significantly high in the ink-sac tissues compared to head and
muscle tissues, except for Pb. The order of heavy metal content in squids is as follows: Zn > Cu > Cd > Pb.
• Compared to the recommended permissible limits, the concentration of Zn and Cu in squid tissues are still
lower than that of safety standards. Meanwhile, the concentration of Cd and Pb are higher than that of safety
standards.
• However, the average value of MPI has shown that the heavy metal concentration in squid tissues is at a low
contamination level (5 < MPI < 10).
ANALYTICAL CHEMISTRY IN MALAYSIA – JOURNAL 2
2) RISK ASSESSMENT OF PHARMACEUTICALLY ACTIVE COMPOUNDS
(PhACs) IN THE KLANG RIVER ESTUARY, MALAYSIA
Introduction
• Pharmaceutically active compounds enter the environment and natural ecosystems through various point sources
such as human waste and sewerage discharge or seepage into water bodies, effluent from wastewater treatment
plants as well as veterinary drugs used in aquaculture activities or that conveyed through the application of
manure and slurry from livestock.
• The ubiquitous presence of PhACs in the environment and especially in aquatic domain has raised concern such
as steroid hormones and synthetic estrogen have been linked to numerous types of adverse health consequences
such as prostate and breast cancer, alteration in male and female reproductive system and changes in
neuroendocrinology, behavior and metabolism.
• Previous studies also reported on the potency of bioaccumulation and biomagnification of PhACs in the aquatic
organisms which can lead to various human and environmental risk.
• Therefore, the present study is carried out to assess the level of selected PhACs contamination in the surface
water of Klang River estuary to evaluate the distribution pattern of PhACs along Klang River estuary and to
calculate the risk assessment associated with the presence of PhACs in the coastal water of Klang River estuary.
• Surface coastal water samples were extracted using offline solid phase, applying polymeric C18 cartridges as
extraction sorbent and measuring with liquid chromatography mass spectrometry–mass spectrometry (LC
MS–MS) technique.
#only for reading purposes
Analytical analysis
• Instrumental analysis was accomplished using Spark Holland liquid chromatography (LC) system equipped with
3200 Q-trap triple quadrupole mass spectrometry (AB Sciex, MA, USA).
• Reversed phase C18 analytical column (Gemini NX, 50 mm 9 2.0 mm, 3 lm, Phenomenex, CA, USA) was used for
separation of compounds in the HPLC system.
• All the pharmaceutical compounds were analyzed in positive ionization mode except diclofenac, which was run on
negative ionization mode.
• For positive ionization mode, formic acid (0.2%, v/v) was added into mobile phase composition, while ammonium
hydroxide (0.2%, v/v) was added into mobile phase composition for negative ionization mode.
• Gradient elution was applied for compounds separation in both ionization modes with mobile phase B being
increased from 5% (initial concentration) to 95% in 4 min and held constant for 2 min, then decreased to the initial
concentration where it was equilibrated for 2 min, for a total run time of 8 min before proceeding for the next run.
• The oven column temperature was fixed at 40 C with the flow rate for mobile phase held at 0.30 mL min-1.
• The injection volume for blank, standards and samples was set at 20.0 lL.
• Mass spectrometry analyzer was operated using following condition: curtain gas, 20 psi; CAD gas 1, 40 psi; CAD
gas 2, 40 psi; temperature, 600 C (positive) and 550 C (negative); ion spray voltage, 4500 V (positive) and 5500 V
(negative).
Further reading: Omar, T. F. T., Aris, A. Z., Yusoff, F. M., & Mustafa, S. (2019). Risk assessment of pharmaceutically active compounds (PhACs) in
the Klang River estuary, Malaysia. Environmental geochemistry and health, 41(1), 211-223.
Result analysis
Introduction
• Plastic pollution has become a controversial environmental issue with a growing concern around the world.
• The small particles (<5 mm) are termed as microplastics (MPs). MPs may pose a potential risk to the
environment due to their tendency to release contaminants such as metals, additives, and UV stabilizers.
• Sungai Dungun has been considerably subjected to various sources of contamination, including urban and
industrial activities, fishing activities, and small-scale agriculture.
• Previous studies showed that this river had experienced deterioration of water quality linked to
phosphate-based nutrients (Suratman et al. 2008), and metals (Aspin 2017).
• In this study, the abundances, distribution, and morphological specificity of microplastics in the surface water
samples from Sungai Dungun, Malaysia was investigated.
#only for reading purposes
Analytical analysis
• MPs were randomly selected for the next analysis using scanning electron microscope (SEM) model
JEOL 6360 LA. Samples were spread on double-sided adhesive tape and coated with a thin film of
evaporated gold. SEM images were taken with an optimised acceleration voltage of 10 kV and a
detector working at distances of approximately 2 mm.
• MPs trapped on the membrane filter, were transferred into the 1.5 mL vial and placed in desiccators for
up to 7 days to completely remove the water content.
• In this study, MP compositions were subject to verification using Fourier transform infrared spectroscopy
(FTIR) analysis, IRTracer-100 (Shimadzu, Japan).
• Metal contents were extracted from MP surfaces using a modified aqua regia extraction.
• Since MP sizes are generally small, MPs trapped on membrane filters were placed in 100 mL beakers.
An amount of 30 mL HCl, 10 mL HNO3 and 10 mL deionised water were added into a beaker and
placed onto a hotplate for 2 h.
• Final concentrations were determined by inductively coupled plasma-optimal emission spectrometry.
Further reading: HWI, T. Y., Ibrahim, Y. S., & Khalik, W. (2020). Microplastic abundance, distribution, and composition in Sungai Dungun,
Terengganu, Malaysia. Sains Malaysiana, 49(7), 1479-1490.
Result analysis
✔ With the drive towards achieving the status of an industry 5.0, the quality of the Malaysian
environment is further threatened.
✔ While the immediate environmental problems, in particular those pertaining to industrial
effluents and sewage, are being addressed by the introduction of integrated treatment
systems such as the proposed central toxic waste plant, future environmental management
strategies need to be considered.
✔ In addition to the installation of appropriate treatment systems, long term solutions will have
to include waste minimization by the introduction of environmentally sound technology as
an integral part of the manufacturing operation, as well as recycling and reuse of effluents
and by-products of treatment systems.
✔ In addition to the regular monitoring of water and air quality by the Department of
Environment, there is a need to undertake measurements of specific chemicals in the
environment as the diversity of industrial effluents increases.
✔ Experience in industrialized nations has shown that the quality of the environment can be
maintained through careful incorporation of environmental considerations into development
programmed.
9.4
FUTURE REQUIREMENTS
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
• Analytical chemistry plays an enormous role in our society, such as in drug manufacturing,
process control in industry, environmental monitoring, medical diagnostics, food production, and
forensic surveys. It is also of great importance in different research areas.
• As the study of the chemical structure and nature of substances, analytical chemistry plays an
important role in the pharmaceutical sciences. But what does the future hold for this burgeoning
field?
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
The development of analytical chemistry in future are expected to be better in certain aspects such as:
1) Miniaturization
In particular, the rise of mobile laboratories and portable benchtop spectrometric devices has enabled
more varied analytical applications of the technology, giving analytical chemists greater scope for
out-of-laboratory work. In the past, most spectrometers were cumbersome instruments that were large
enough to fill a room. Today, a Raman spectrometer can fit inside a chemist’s pocket and be integrated
with smartphones for monitoring.
With greater miniaturization, analytical chemists will be able to use spectrometric devices in ways that not
have been thought possible a decade ago.
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
2) Automated analysis
In recent years, the automation of analytical instruments (such as autosamplers,
databases, data treatment, and control of instruments using microprocessors) has
accelerated the advancement of analytical chemistry techniques.
Automation has long been employed to solve a number of industrial and laboratory
problems. In the chemical and petroleum industry, these automatic analytical systems are
typically based on gas chromatography, a technique used for separating and analyzing
compounds that can be vapourised without decomposition.
In metallurgical plants, similar systems such as fast sampling tools, pneumatic mail for
transporting samples to a laboratory, and atomic emission spectrometers are already in
use.
In the laboratory, automatic systems for analysis often include continuous flow
(particularly in the agriculture and pharmaceutical industries) or flow injection analysis.
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
Improvements in software and computational technology have also led to the generation
of ever-expanding data sets that need to be sorted, stored and analyzed. As such,
analytical chemists working with these complex data sets need to be well versed in
statistics and chemometrics, as well as being a specialist in sampling, instrumentation,
and interpretation.
The use of laboratory robots is also on the rise, with some fears that the advent of
robotics may kill this traditionally hands-on discipline. However, the vast amounts of data
generated by modern techniques and instrumentation actually represent an opportunity
for analytical chemists because their cognitive skills are needed to render the data useful.
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
The direct knock-on effect of the developments explored above is a cheaper and faster end-to-end
research process.
More advanced separation techniques and the increasing use of computer simulation modelling removes
the need for additional experiments, helping to save time and money. Specific method development and
optimisation software programmes such as DryLab, for example, can even enable researchers to predict
chromatograms using a small number of data points.
As analytical instruments and protocols become more advanced, it will also become possible to perform
complex analytical tasks with higher sensitivity and greater accuracy.
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
Ultra-Performance Liquid Chromatography (UPLC), for example, offers a more accurate analysis than
traditional High-Performance Liquid Chromatography (HPLC) due to its higher throughput and
enhanced ability for separation.
For this reason, the use of UPLC and other hyphenated techniques have become increasingly
commonplace in certain industries, particularly the pharmaceutical sector.
Currently, multidimensional gas techniques such as GCxGC and LCxLC are widely used in a range of
industries, while developments are taking place in column technology and mass spectrometry.
Another emerging area is tandem mass spectrometry (MS/MS), a technique in which two or more
mass spectrometers are coupled up to better analyze chemical samples.
For example, MS could be coupled with polymerase chain reaction (PCR) techniques to rapidly identify
genetic biomarkers for personalized medicine and diagnosis of many non-infectious diseases. New MS
technology will enable us to undertake quantitative analysis of the protein expression patterns
associated with many cancers for more rapid diagnosis.
WHAT IS THE FUTURE OF ANALYTICAL CHEMISTRY?
As is the case across all areas of scientific research, sustainability is becoming a key theme in
analytical chemistry.
Green analytical chemistry is an emergent field that focuses on minimizing the consumption of
dangerous substances, as well as maximizing safety both for operators and the environment.
The miniaturization of equipment and procedures also forms a key part of sustainable analytical
chemistry strategies.
END OF
CHAPTER
THANK YOU