Spotlight on Analytical Applications e-Zine - Volume 11

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SPOTLIGHT
ON APPLICATIONS.
FOR A BETTER
TOMORROW.

VOLUME 11

CONTENTS
TABLE OF

INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 11
PerkinElmer knows that the right training, methods and application support are
as integral to getting answers as the instrumentation. That’s why PerkinElmer has
developed a novel approach to meet the challenges that today’s labs face, delivering
you complete solutions for your application challenges.

We are pleased to share with you our Spotlight on Applications e-zine, which
delivers a variety of topics that address the pressing issues and analytical challenges
you may face in your application areas today.

Our Spotlight on Applications e-zine consists of a broad range of applications
you’ll be able to access at your convenience. Each application in the table of
contents includes an embedded link which that take you directly to the appropriate
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CONTENTS
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CONTENTS

Energy & Industrial
• mproved HyperDSC Method to Determine Specific Heat Capacity of Nanocomposites and
I
Probe for High-Temperature Devitrification
• Polymer Identification Using Mid Infrared Spectroscopy
• n Introduction to Flow Field Flow Fractionation and Coupling to ICP-MS
A
• oupling Flow Field Flow Fractionation to ICP-MS for the Detection and Characterization
C
of Silver Nanoparticles

Environmental
• he Determination of Low Levels of Benzene, Toluene, Ethyl Benzene and Xylenes (BTEX) in
T
Drinking Water by Headspace Trap GC/MS
• mproved Sensitivity and Dynamic Range Using the Clarus SQ 8 GC/MS System for EPA Method
I
8270D Semi-Volatile Organic Compound Analysis

Food Beverage
• Qualifying Mustard Flavor by Headspace Trap GC/MS using the Clarus SQ 8
• imultaneous Analysis of Nine Food Additives with the PerkinElmer Flexar FX-15 System
S
Equipped with a PDA Detector
• nalysis of Pb, Cd and As in Spice Mixtures Using Graphite Furnace Atomic Absorption
A
Spectrophotometry
• Practical Food Applications of Differential Scanning Calorimetry (DSC)

Forensics Toxicology
• piates in Urine by SAMHSA GC/MS
O
• haracterization of Single Fibers for Forensic Applications Using High Speed DSC
C

Pharmaceuticals Nutraceuticals
• nalysis of Drug Substances in Common Cold Medicines with the PerkinElmer
A
Flexar FX-15 System Equipped with a PDA Detector
• etection and Quantification of Formaldehyde by Derivatization with
D
Pentafluorobenzylhydroxyl Amine in Pharmaceutical Excipients by Static Headspace GC/MS

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a p p l i c at i o n n o t e

Differential Scanning Calorimetry

Authors
Bruce Cassel1
Andrew Salamon1
E. Sahle-Demessie2
Amy Zhao2
Nicholas Gagliardi3
1 PerkinElmer, Inc.
Shelton, CT, USA
2 U.S. Environmental Protection Agency
Cincinnati, OH, USA
3 University of Dayton Research Institute
Dayton, OH, USA

Improved HyperDSC Introduction
There has been tremendous interest in
Method to Determine recent years in nanocomposites – using
small scale particulate fillers – to improve
Specific Heat Capacity the properties of thermoplastics and
thermosets. For example, the effect of
of Nanocomposites and using such small scale filler particles is
such as to toughen the plastics, reduce
Probe for High-Temperature vapor transfer, and improve transparency.
One rapid way to quantify the effect
Devitrification of a particular filler formulation is to
measure its effect on the change in
specific heat (Cp) that occurs at the
glass transition (Tg). In this analysis, discussed by Christophe Schick,1 the Cp of
an amorphous nanocomposite can be usefully partitioned between three entities:
(1) unaffected amorphous polymer whose properties are the same as that in the
pure amorphous polymer, called the mobile amorphous fraction; (2) the Cp of
the filler itself; and (3) the Cp of the polymer which is immobilized by its attachment
to the nanoparticle, the rigid amorphous fraction (RAF). The properties of the
composite can be related to the extent of these fractions. The chemical bonding
– weak or strong – of the RAF to the nanomaterial filler may be an indicator of
the performance of the nanocomposite, and it may be an indicator of how readily
it will decompose in the environment. A second Tg – devitrification of the RAF –
would indicate a relatively weak bond of the RAF to the nanomaterial filler.

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Infrared Spectroscopy

Polymer Identification Introduction
Synthetic polymers are very widely used
Using Mid Infrared today, with diverse applications in various
industries such as food, automotive, and
Spectroscopy packaging. The quality of plastic products
depends on the quality of the polymers or
polymer blends used during manufacturing,
so identity verification and quality testing of those materials during every stage
of manufacturing is necessary to ensure that only high-quality material is used.

Infrared (IR) spectroscopy is ideally suited to qualitative analysis of polymer starting
materials and finished products as well as to quantification of components in
polymer mixtures and to analysis of in-process samples. IR spectroscopy is reliable,
fast and cost-effective. This application note describes several approaches to the
measurement and analysis of IR spectra of typical polymer samples, and applies
the techniques to the identification of some industrial polymer samples. The
compact and rugged Spectrum Two™ FT-IR spectrometer supports a range of
reflectance and transmission sampling accessories that are suitable for polymer
analysis, and is now available with a Polymer Resource Pack that provides infor-
mation and advice to help generate good quality spectra and extract meaningful
information as simply as possible.


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White
paper Inductively Coupled Plasma – Mass Spectrometry

Authors
Denise Mitrano
James F. Ranville
Department of Chemistry and Geochemistry
Colorado School of Mines
Golden, CO USA
Kenneth Neubauer
Senior Scientist – ICP-MS Technology
PerkinElmer, Inc.
Shelton, CT USA

An Introduction to
Flow Field Flow Introduction
Inductively coupled plasma-mass spectrometry
Fractionation and (ICP-MS) is the method of choice for analysis
of most elements across the periodic chart.
Coupling to ICP-MS Its multi-element capability, low detection
limit (ppt), and wide dynamic range (109
orders of magnitude) also make it ideal for
the measurement of inorganic engineered nanoparticles (ENPs). While ICP-MS
can be used directly to obtain concentrations of nanoparticulate-associated
elements, more information on characteristics of ENPs can be obtained by first
separating the particles by size prior to ICP-MS analysis. The most versatile
size-separation technique is field flow fractionation (FFF). By introducing size-
fractionated material into the ICP-MS, the size and elemental composition of
complex, polydisperse and chemically heterogeneous ENPs can be determined.
Furthermore, the similar flow conditions required by both ICP-MS and FFF make
interfacing relatively simple.

Field Flow Fractionation
Field flow fractionation (FFF) consists of a suite of high-resolution elution techniques
which can size separate nanoparticles in the 1-100 nm range and colloids up
to 1 micron. By use of either FFF theory or calibration with size standards, the
technique can be utilized to determine particle size. The separation process is
similar to chromatography except that the separation is based on physical
forces as opposed to chemical interactions.

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ICP-Mass Spectrometry

Authors
Denise Mitrano
James F. Ranville
Department of Chemistry and Geochemistry
Colorado School of Mines
Golden, CO USA
Kenneth Neubauer
Senior Scientist – ICP-MS Technology
PerkinElmer, Inc.
Shelton, CT USA

Coupling Flow Field Introduction
Analysis of nanomaterials should include characterization
Flow Fractionation of composition as well as size. Many techniques are
capable of sizing nano-size particles, such as dynamic
to ICP-MS for the light scattering (DLS), UV/Vis spectrophotometry, and
transmission electron microscopy (TEM), yet provide
Detection and no information on the composition of the particle
and/or are time intensive and costly. Inductively coupled
Characterization of plasma-mass spectrometry (ICP-MS), however, is a
standard instrument in many analytical laboratories
Silver Nanoparticles and is the method of choice for analysis of most
elements across the periodic chart. The multi-element
capability of the ICP-MS, low detection limit (ppt),
and wide dynamic range (109 orders of magnitude) also make it ideal for application to
the measurement of inorganic engineered nanoparticles (ENPs). While ICP-MS can be used
directly to obtain concentrations of nanoparticulate-associated elements, more information
on characteristics of ENPs can be obtained by coupling a size-separation step prior to
ICP-MS analysis. The most versatile size-separation technique for this application is field
flow fractionation (FFF). Although FFF is a powerful nanoparticle sizing technique, many
common detectors used in conjunction with FFF do not provide the needed compositional
information of the particles. Therefore, the resultant hyphenated technique of FFF-ICP-MS
provides nanoparticle sizing, detection, and composition analysis capabilities at the parts
per billion (ppb) level, which is critical to environmental investigations of nanomaterials.
Furthermore, the similar flow conditions required by both ICP-MS and FFF make interfacing
relatively simple.


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Gas Chromatography/
Mass Spectrometry

Author
Lee Marotta
PerkinElmer, Inc.
Shelton, CT 06484 USA

The Determination of Introduction
BTEX is a grouping of structurally similar
Low Level Benzene, volatile organic compounds including
benzene, toluene, ethyl benzene and the
Toluene, Ethyl Benzene, three xylene isomers. These compounds
are known pollutants and are typically
and Xylenes (BTEX) found near petroleum production and
storage sites. BTEX are regulated toxic
in Drinking Water by compounds while benzene is also an EPA
target carcinogen. The investigation of
Headspace Trap GC/MS these compounds, especially in drinking
water at low levels, is critical to protect
public health. This application note focuses
on exceeding the current EPA detection limit requirement for BTEX while meeting
and/or exceeding all other criteria in EPA method 524.2 for these analytes.

Instrumentation
A PerkinElmer® TurboMatrix™ Headspace (HS) sample handling system was used
to volatilize and concentrate BTEX in water samples. To enhance detection limits, an
inline trap was employed, which focused these analytes prior to injection onto
the analytical column. A PerkinElmer Clarus® SQ 8S Gas Chromatograph Mass
Spectrometer (GC/MS) configured with the standard capacity turbo molecular pump
was the analytical system used.


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Gas Chromatography/
Mass Spectrometry

Authors
Yury Kaplan
Ruben Garnica
PerkinElmer, Inc.

Improved Sensitivity Introduction
U.S. Environmental Protection
and Dynamic Range Agency (EPA) Method 8270D – Semi-
Volatile Organic Compounds by Gas
Using the Clarus SQ 8 Chromatography/Mass Spectrometry
(GC/MS) – is a common and wide ranging
GC/MS System for method employed in nearly all commercial
environmental laboratories. The analysis
EPA Method 8270D focuses on the detection of trace level
semi-volatile organic compounds in
Semi-Volatile Organic extracts from solid waste matrices, soils,
air sampling media and water samples.
Compound Analysis The method lists over 200 compounds
however a majority of laboratories target
between 60 and 90 for most analyses.
The study presented here demonstrates
the PerkinElmer® Clarus® SQ 8 GC/MS, not only meets the method requirements
but provides users flexibility to satisfy their individual productivity demands.
An extended calibration range is presented as are the advantages of the Clarifi™
detector.


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Gas Chromatography/
Mass Spectrometry

Author
Ruben Garnica
Andrew Tipler
PerkinElmer, Inc.

Qualifying Mustard Mustard is a common condiment used across many cultures
and culinary styles to enhance the dining experience. It

Flavor by Headspace is derived from the mustard seed and is used either as a
dried spice, spread or paste when the dried spice is mixed

Trap GC/MS using with water, vinegar or other liquid. The characteristic
sharp taste of mustard arises from the isothiocyanates
the Clarus SQ 8 (ITCs) present as result of enzymatic activity made possible
when the ground seed is mixed with liquids. The focus of
this application brief is the characterization of these ITCs
by headspace trap gas chromatography/mass spectrometry
(GC/MS) and a qualitative description of their relationship
to sharpness in taste across various mustard products.


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UHPLC

Author
Njies Pedjie
PerkinElmer, Inc.

Simultaneous Analysis of Introduction
Food additives are natural or synthetic
Nine Food Additives with substances that are added in food,
beverage and pharmaceutical products
the PerkinElmer Flexar for their microbicidal, preservative and
flavoring properties. Among the commonly
FX-15 System Equipped used additives, benzoic acid and its salts
are widely used in beverage and food
with a PDA Detector for preservation. Artificial sweeteners
are widely used as sugar substitute in
calorie-conscious societies, where their
intake provides practically no calories and
also helps fight obesity and its related
ailments.

In most countries, the use of additives is regulated. In the U.S., most additives
are part of the Generally Recognized As Safe (GRAS) ingredients although the
FDA has established Acceptable Daily Intake (ADI) for each of them. There is
a need for analytical techniques to identify and quantify additives because the
food industry is required to list the type and amount of each ingredient on product
labels to help consumers make dietary choices and manage food allergies.

This application note presents a fast and robust liquid chromatography method
to simultaneously test nine widely used additives. Among the additives tested
are: preservatives (benzoic acid, sorbic acid, dehydroacetic acid and methylparaben);
artificial sweeteners (acesulfame potassium, saccharin and aspartame); flavoring
agent (quinine); and a stimulant (caffeine). Method conditions and performance
data including precision, accuracy and linearity are presented. The method is
applied to a mouthwash and a tonic soda and the type and amount of additives
are confirmed.


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Atomic Absorption

Author
Praveen Sarojam, Ph.D.
PerkinElmer, Inc.

Analysis of Pb, Cd and Introduction
The toxicity and effect of trace heavy metals on
As in Spice Mixtures human health and the environment has attracted
considerable attention and concern in recent years.
using Graphite Furnace With an inherent toxicity, a tendency to accumulate
in the food chain and a particularly low removal rate
Atomic Absorption through excretion,1 lead (Pb), cadmium (Cd) and
arsenic (As) cause harm to humans even at low
Spectrophotometry concentrations. Exposure to trace and heavy metals
above the permissible level affects human health and
may result in teratogenicity (reproductive effects).
Individuals may also experience high blood pressure,
fatigue, as well as kidney and neurological disorders.

Spices, the dried parts of plants, grow widely in various regions of the world, are produced
either on small farmlands or naturally grown, and have been used for several purposes since
ancient times. Most are fragrant and flavorful and are used for culinary purposes to improve
the quality of food.2 Natural food spices, such as pepper, have been reported to contain
significant quantities of some heavy metals, including Pb, Cd and As. Contamination with
heavy metals may be accidental (e.g. contamination of the environment during plant
cultivation) or deliberate – in some cultures, according to traditional belief, specially treated
heavy metals are associated with health benefits and are thus an intentional ingredient of
traditional remedies. Spices and herbal plants may contain heavy metal ions over a wide
range of concentrations.3,4 There is often little information available about the safety of
those plants and their products in respect to heavy metal contamination. Due to the
significant amount of spices consumed, it is important to know the toxic metal
concentrations in them.5


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Authors
Patricia Heussen
Unilever
Research Development
Vlaardingen, The Netherlands

Peng Ye, Kevin Menard, Patrick Courtney
PerkinElmer, Inc.

Practical Food Applications of
Differential Scanning Calorimetry (DSC)
Abstract
This note describes a number of important food applications utilising the PerkinElmer DSC demonstrating
the versatility of the technique as a tool in the food industry.

Introduction
Food is often a complex system including various compositions and structures. The characterization
of food can therefore be challenging. Many analytical methods have been used to study food,
including differential scanning calorimetry (DSC).1 DSC is a thermal analysis technique to measure
the temperature and heat flows associated with phase transitions in materials, as a function of
time and temperature. Such measurements can provide both quantitative and qualitative informa-
tion concerning physical and chemical changes that involve endothermic (energy consuming) and
exothermic (energy producing) processes, or changes in heat capacity.

DSC is particularly suitable for analysis of food systems because they are often subject to heating
or cooling during processing. The calorimetric information from DSC can be directly used to under-
stand the thermal transitions that the food system may undergo during processing or storage. DSC
is easy to operate and in most cases no special sample preparation is required. With a wide range
of DSC sample pans available, both liquid and solid food samples can be studied. Typical food
samples and the type of information that can be obtained by DSC are listed in Table 1. These tests
can be used for both QC and RD purposes. DSC applications are used from troubleshooting up to
new product developments.


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Gas Chromatography/
Mass Spectrometry

Author
Timothy D. Ruppel
PerkinElmer, Inc.

Opiates in Urine by Introduction
The United States Department of Health and Human Services
SAMHSA GC/MS (DHHS), Substance Abuse and Mental Health Services Administration
(SAMHSA) regulates urine drug testing programs in the mandatory
guidelines for the Federal Workplace Drug Testing Program. These
Mandatory Guidelines require a laboratory to conduct two analytical
tests before a urine specimen can be reported positive for a drug, the
initial drug test and the confirmatory drug test. The initial drug test
is performed by immunoassay screening for the five drug classes
(i.e., amphetamines, cocaine, opiates, phencyclidine, and marijuana).
Examples of immunoassay screening would include radioimmunoassay
(RIA), enzyme immunoassay (EIA, EMIT) or others.

Samples found positive to the immunoassay screening are subjected
to a second confirmatory test by chromatographic separation and
identification by mass spectrometry. SAMHSA defines the method
quantification cutoff level as 2000 ng/mL each for codeine and morphine.
If morphine is detected above 2000 ng/mL, then an additional
quantification for 6-acetylmorphine is suggested. 6-AM is a unique
metabolite indicating the use of heroin. 6-AM cutoff level is 10 ng/mL.


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Characterization of Introduction
Crime or forensic laboratories must frequently work with very small
Single Fibers for samples in order to determine the type of material and its possible
manufacturer for investigatory and evidence purposes. An example
Forensic Applications would be in the characterization of single fibers found at the crime
scene. Fibers are useful for forensic purposes, as they tend to cling
Using High Speed DSC easily and provide useful characteristics for identification purposes.
The disadvantage is the fibers are very low-mass (on the order of
50 µg) which renders it difficult for thermal analysis characterization
techniques.

Thermal analysis, and in particular Differential Scanning Calorimetry
(DSC), is useful for characterizing polymers and fibers. Typically,
the mass used for DSC experiments is at the order of 5 to 10 mg.
However, a single fiber has a mass that is 100 times less than the
usual weight. For this special application, a DSC instrument with a
high level of sensitivity and performance is required. In particular,
High Speed DSC is a very useful approach for the characterization
of low-mass materials since the use of very fast heating rates (100
to 400 ˚C/min) provides significantly greater sensitivity. Power
Compensation DSC has been successfully used for forensic studies
of toners on photocopied documents.1
DSC 8500


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UHPLC

Author
Njies Pedjie
PerkinElmer, Inc.
Shelton, CT USA

Analysis of Drug
Substances in Common
Cold Medicines with
the PerkinElmer Flexar Introduction
The common cold is a frequent upper respiratory
FX-15 System Equipped tract infection caused by a number of different
types of viruses. Common cold affects billions of
with a PDA Detector people worldwide every year; its typical symptoms
include a runny nose, nasal congestion and sneezing.
Colds can also cause sore throat, cough and
headache. Common cold viruses do not respond to antibiotics and there are no known
cures. Although the symptoms are normally resolved within ten days, they can cause a
great deal of discomfort. Fortunately, these symptoms can be alleviated by the use of
over-the-counter medicines. These cold remedies invariably include acetaminophen (a
pain reliever and fever reducer), a cough suppressant (antitussive) and a nasal decon-
gestant. Commonly used antitussive and nasal decongestant are dextromethorphan HBr
and phenylephrine HCL. Dextromethorphan temporarily relieves cough by decreasing
activity in the part of the brain that causes the coughing. Phenylephrine relieves nasal
discomfort and sinus congestion by reducing the swelling of blood vessels in the nasal
passages. Since they don’t treat the underlying cause of the illness, cold medicines do
not necessarily speed the recovery.


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Gas Chromatography/
Mass Spectrometry

Author
Padmaja Prabhu
PerkinElmer, Inc.
Shelton, CT USA

Detection and Quantification of Introduction
Although considered pharmacologically
Formaldehyde by Derivatization inert, pharmaceutical excipients have been
with Pentafluorobenzylhydroxyl shown to interact with active drug sub-
stances to affect the safety and efficacy
Amine in Pharmaceutical Excipients of drug products.1 Therefore, there is an

by Static Headspace GC/MS increasing awareness of the necessity
to understanding interactions between
excipients and the active pharmaceutical
ingredient (API) in finished dosage forms.
One of the areas of major concern is the potential chemical interaction between
impurities in the excipient with the drug molecules, leading to formation of reaction
products.2 Even trace amounts of reactive impurities can cause significant drug
stability problems as the quantity of excipients in a formulation often far exceeds
that of an API on a weight and molar basis. Trace amounts of reaction products
can then easily exceed 0.2% qualification thresholds for a degradation in many
drug products.1 Formaldehyde present in excipients has been implicated in the
Figure 1. Structure and
degradation of several drug products where it can form adducts with primary and/
properties of formaldehyde. or secondary amine groups.2 It has also been reported that formaldehyde can
induce cross-linking in gelatin capsules causing an adverse effect on in-vitro
dissolution rates of drugs. Because of the extremely high reactivity of aldehydes,
a timely evaluation of their presence in excipients during formulation design is
essential to avoid unexpected drug stability problems in later stages of product
development.


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USEFUL LINKS
View previous issues of our Spotlight on Applications e-Zine
• Volume 1 • Volume 4 • Volume 7 • Volume 10
• Volume 2 • Volume 5 • Volume 8 • Archives
• Volume 3 • Volume 6 • Volume 9

Access our application archives
By Industry:
• Consumer Products
• Energy
• Environmental
• Food, Beverage Nutraceuticals
• Forensics
• Lubricants
• Pharmaceutical Development Manufacturing Environmental Disasters:
• Polymers/Plastics
• Semiconductor Electronics Be Prepared with Critical Testing
Insights from Past Experiences:
By Technology: View the webcast and hear from the experts
• Atomic Absorption (AA)
• Elemental Analysis
• Gas Chromatography (GC)
• GC Mass Spectrometry (GC/MS)
• Hyphenated Technology
• ICP Mass Spectrometry (ICP-MS)
• Inductively Coupled Plasma (ICP-OES ICP-AES)
• Infrared Spectroscopy (FT-IR IR)
• LIMS Data Handling
• Liquid Chromatography (HPLC UHPLC)
• Mass Spectrometry
• Raman Spectroscopy
• Thermal Analysis
• UV/Vis UV/Vis/NIR

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