PerkinElmer Spotlight on Analytical Applications e-Zine – Volume 16

VOLUME 16
SPOTLIGHT
ON APPLICATIONS.
FOR A BETTER
TOMORROW.
TABLE
OF
CONTENTS

PerkinElmer
TABLE
OF
CONTENTS
INTRODUCTION
PerkinElmer Spotlight on Applications e-Zine – Volume 16
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 takes you directly to the appropriate page within the e-zine.
We invite you to explore, enjoy and learn!
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PerkinElmer
CONTENTS
TABLE
OF
CONTENTS
Environmental
• The Analysis of Water and Wastes by U.S. EPA Method 200.7 Using the Optima 8300 ICP-OES
and prepFAST Auto-Dilution/ Calibration System
• The Measurement of Fullerene C-60 using DSA TOF
Consumer Products
• Screening for Paraben in Texture Cream using DSA TOF
• Detecting Salicylic Acid in Foundation through DSA TOF
Food & Beverage
• Arsenic Speciation Analysis in Brown Rice by HPLC/ICP-MS
• Rapid Measurement of Olive Oil Adulteration with Soybean Oil with Minimal Sample
Preparation Using DSA/TOF
• Arsenic Speciation Analysis in White Rice by HPLC/ICP-MS
• Targeted Screening of 130 Pesticides in QuEChERS Extracts of Lettuce Leaves Using UHPLC-TOF
and High Throughput Screening Software
Pharmaceuticals & Nutraceuticals
• Quantitation of the Amorphicity of Lactose Using Material Pockets
• Implementation of USP New Chapters <232> and <233> on Elemental Impurities
in Pharmaceutical Product
Forensics and Toxicology
• The Benefits of NexION 300D ICP-MS’ Reaction Mode in Removing the Gd+2 Interference
on Selenium in Serum
• The Advantages of the NexION 300D ICP-MS for the Determination of Titanium in Serum

TABLE
OF
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TOF MS
DIRECT SAMPLE ANALYSIS
Chemical: Paraben Screening in Texture Cream
Easy to use
Ensures product safety
No sample prep
• DSA/TOF allowed for fast screening
of paraben-free texture cream and
confirmed the absence of parabens
with high mass accuracy
• The analysis was performed in 15
seconds with no sample preparation
• Parabens are a class of chemicals used in
preservation of personal care products
and are implicated to negatively impact
human health
• Traditional sample preparation and
method development of parabens is
time consuming, approximately 25 min
per sample.
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010884_01
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TOF MS
Chemical: Salicylic Acid in Foundation
Results in seconds
Product integrity
No sample prep or
chromatography
• DSA/TOF direct analysis of foundation
confirms the presence of salicylic acid
with accurate mass
• The analysis was performed in 15
seconds with no sample preparation
• Salicylic acid is a common ingredient in
acne fighting personal care products used
to help clear and prevent skin blemishes
• Liquid foundation was directly
analyzed to determine if salicylic acid
was present

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A P P L I C A T I O N N O T E
Authors:
Deborah K Bradshaw
Atomic Spectroscopy
Training and Consulting
Laura Thompson
PerkinElmer, Inc.
Shelton, CT
Introduction
The prevention and control of
water pollution is of critical
importance to protecting human
and environmental health.
Monitoring of water and wastes
is an efficacious way to prevent
the introduction of pollutants
and costly remediation of
drinking and environmentally
important waters. The United States Environmental Protection Agency (U.S.
EPA), along with local regulatory bodies, is responsible for regulating water
and wastes under the Clean Water Act and the Safe Drinking Water Act.
Depending on the number and type of analytes, the number of samples and
the productivity requirements, several different analytical techniques can be
applied to measure trace elements in water and wastes.
U.S. EPA Method 200.7 Version 4.4 covers the use of inductively coupled
plasma optical emission spectroscopy (ICP-OES) in radial and/or axial viewing
for the determination of metals and some non-metals in water and wastes
for regulatory compliance.1
Method 200.7 contains a lengthy description of
procedures for the collection, preservation and preparation of samples for
analysis. The objective of this work was to complete the method using the
PerkinElmer®
Optima®
8300 ICP-OES coupled with the prepFAST™ Automated
In-Line Auto-Dilution/Calibration System (Elemental Scientific Inc., Omaha, NE).
The Analysis of Water
and Wastes by U.S. EPA
Method 200.7 Using the
Optima 8300 ICP-OES and
prepFAST Auto-Dilution/
Calibration System
ICP-OpticalEmissionSpectroscopy

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010564_01
PerkinElmer, Inc.
940 Winter Street
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
TOF MS
Easy to use
No chromatography
Fast accurate mass
Chemical: Fullerene C-60
• The analysis was performed in
15 seconds with no sample preparation
and external calibration
• DSA/TOF analysis, in negative mode,
of a 1 mg/mL fullerene C-60 in toluene
• Buckminster fullerenes are researched
for their technological applications in
materials science and nanotechnology.

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Introduction
Arsenic (As) is a well-known toxic element
which has been highly regulated, especially
for drinking water. Although regulatory limits
have been for total arsenic, its toxicity varies widely and is dependent on its chemical
form. For example, inorganic forms of arsenic are highly toxic and carcinogenic.
However, organic forms (such as monomethylarsonic acid, dimethylarsinic acid, and
arsenobetaine) are recognized as non-toxic or as having low toxicity.
The Joint Expert Committee on Food and Additives (JECFA) recognizes the importance
of monitoring inorganic arsenic intake. In 1988, they established a provisional
tolerable weekly intake (PTWI) of 0.015 mg/kg body weight inorganic arsenic.
However, this recommendation was withdrawn in 2010.
In Japan, the average total arsenic intake/person/day is divided between seafood
(53.6%), vegetables and seaweed (35.4%), rice (7.1%), and other sources.1
It is known that the majority of arsenic in marine organisms is in the form of
arsenobetaine, which is non-toxic. However, because of the large quantities of rice
consumed in Japan, it is important to know what forms of arsenic are present in rice.
Arsenic Speciation
Analysis in Brown Rice
by HPLC/ICP-MS
HPLC/ICP-MS
Authors:
Kyoko Kobayashi, Osamu Shikino
Inorganic Product Specialists
PerkinElmer Japan Co., Ltd.

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Introduction
Among edible oils, olive oil shows
important and outstanding characteristics
due to its differentiated sensorial qualities
(taste and flavor) and higher nutritional
value. It is an important oil that is high in
nutritional value due to its high content
of antioxidants (including vitamin E)1
.
Several health benefits, such as its ability to lower LDL cholesterol and
its anti-inflammatory activity, associated with its consumption were
initially observed among Mediterranean people2,3
. Olive oil is one of the
most adulterated food products of the world due to its relatively low
production and higher prices as compared to vegetable and seed oils.
Rapid Measurement of
Olive Oil Adulteration
with Soybean Oil with
Minimal Sample
Preparation Using
DSA/TOF
Mass Spectrometry
Author:
Avinash Dalmia
George L. Perkins
PerkinElmer, Inc.
Shelton, CT USA

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HPLC/ICP-MS
Authors:
Jong Min Park, Sang Kwon Ma
Inorganic Product Specialists
PerkinElmer South Korea
Introduction
There has been a rising concern
about the presence of arsenic in
rice, especially in societies which
consume large quantities of rice. Arsenic can enter rice naturally through the
environment or through the application of pesticides. Because not all arsenic
species are toxic, the ability to measure the different forms is important.
In recent years, it has become common to measure different forms of arsenic
using HPLC/ICP-MS: HPLC separates the forms and ICP-MS detects them as
they elute from the column. The advantage of ICP-MS as an HPLC detector
is that it is very sensitive and can measure trace levels, as demonstrated by
its use to measure impurities in a wide range of electronic materials and
environmental samples.
This work demonstrates the ability to measure various arsenic forms in white
rice, building upon previous work.1,2
Arsenic Speciation
Analysis in White Rice
by HPLC/ICP-MS

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Introduction:
The Food Quality protection Act (FQPA) in the United States (US)
and the European Union (EU) directive 91/414/EEC require that
if pesticides are present in food they are below agreed levels
due to the health risk posed by pesticides 1, 2
. With the advent of
large scale agricultural production, hundreds of pesticides have
been synthesized in the last century and used widely to protect
crops. Newer pesticides continue to be synthesized for crop usage
which makes it important to analyze both targeted (or expected
analytes) and non-targeted pesticides in food and in the environment. Unlike a triple
quadrupole instrument that only measures targeted analytes (defined by selected multiple
reaction monitoring of analyte ions or MRMs), the time-of-flight (TOF) mass spectrometer
can measure both targeted and non-targeted analytes3
. TOF mass spectrometers collect
full spectrum information and hence the data can be re-examined for the presence of
these “non-targeted” analytes. We present a study of pesticide analysis in a lettuce
leaves extract that was obtained by the QuEChERS (Quick, Easy, Cheap, Effective,
Rugged and Safe) method of food extraction. The lettuce extract was spiked with varying
concentrations of a mix of 130 pesticides and analyzed by Ultra-High Pressure Liquid
Chromatography-Mass Spectrometry (UHPLC-MS) with a PerkinElmer AxION®
2 TOF MS
as the detector. We could detect the majority of the pesticides well within the EU limit of
detection (LOD) requirement range of 10 ppb. The data was further analyzed using AxION
SoloTM
high throughput software. The presence of each of the analytes when detected
above the 10 ppb threshold was given a specific color code which helped to rapidly
screen for presence/absence of all 130 analytes in each sample. A combination of short
run times and powerful screening software helped simplify analysis and also reduce the
time of analysis.
Liquid Chromatography/
Mass Spectrometry
Authors:
Sharanya Reddy
Ariovaldo Bisi
PerkinElmer, Inc.
Targeted Screening of 130
Pesticides in QuEChERS
Extracts of Lettuce Leaves
Using UHPLC-TOF and
High Throughput
Screening Software

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Introduction
The analysis of bodily fluids for trace
elements is common to monitor
individuals’ exposure to toxic elements
and assess nutritional deficiencies.
To realize these goals, urine, whole
blood, and blood serum are commonly
analyzed for a variety of trace elements.
Although these matrices are similar,
there could be wide variation within
a matrix type among individuals. This work describes a case study involving the
analysis of selenium in blood serum, where the ability to remove the gadolinium
(Gd) doubly-charged interference is demonstrated.
Experimental
Sample Preparation
Ten serum samples and two QC samples (UTAK Serum, Normal and High) were
prepared by 10x dilution in 1% nitric acid. Germanium (10 µg/L) was added as an
internal standard. Quantitative results were determined with Additions Calibrations,
which involves preparing the calibration standards in a representative sample and
measuring all other samples against this calibration curve.
ICP-MS
Authors
Peter Dickenson1
, Gavin Robinson2
1
PerkinElmer Australia
Melbourne, Victoria 3150
Australia
2
Robinson Scientific
Cambridge 3434
New Zealand
The Benefits of
NexION 300D ICP-MS’
Reaction Mode in
Removing the Gd+2
Interference on
Selenium in Serum

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TABLE
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A P P L I C A T I O N B R I E F
ICP-Mass Spectrometry
Introduction
Titanium (Ti) is commonly used in
metallic hip replacement joints.
Owing to wear and tear or
different types of electrochemical
processes that could take place in
the body, there is a serious potential of leakage of Ti into the surrounding
tissues. As such, it is important to monitor the Ti serum levels in patients
that have undergone or are due to undergo a hip replacement surgery. The
analysis of Ti in serum by inductively coupled plasma mass spectrometry
(ICP-MS) faces many challenges due to significant spectroscopic
interferences from Ca on the major isotope of Ti (m/z 48) and other
molecular ions such as PO+
, SO+
, CO2
+
, ArC+
and NO2
+
.
The PerkinElmer NexION®
300D ICP-MS is a robust, highly innovative
cell-based system benefitting from three quadrupoles with the middle
one acting as a universal cell. This cell can be used both as a collision cell
using inert gases, such as He, and as a true dynamic reaction cell with
the benefits of using the most appropriate reactive gas for the efficient
targeting of any spectral interference. In this work, we describe a method
to shift the Ti ions away from the interferences using Reaction mode with
ammonia as the reaction gas to determine the concentration of Ti in serum.
The Advantages of the
NexION 300D ICP-MS
for the Determination
of Titanium in Serum
Authors:
Fadi Abou-Shakra
David Price
PerkinElmer, Inc.
Shelton, CT

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Summary
Lactose is a very important pharmaceutical excipient used in tablet and
inhalation products. It is prone to forming amorphous regions on processing
however, and can be problematical to characterize the exact amount of
amorphic material in a sample. This application note describes a DMA
method for quantitatively determining the amorphic content of lactose
using the PerkinElmer®
Material Pocket. The complex tan δ response will
be interpreted and an indication of the detection limits of the technique
will be discussed.
Introduction
Dynamic Mechanical Analysis (DMA) is one of the most appropriate methods
to investigate relaxation events. This fact, until now, has not been
exploited for powdered materials due to the difficulty in handling them in
mechanical tests. The Material Pocket was developed to allow powdered
materials to be investigated in a DMA 8000. The size of the observed
glass transition in the tan δ response is directly proportional to the
amount of amorphous material in the sample. As the crystalline component
has no glass transition, it has no contribution to the result obtained.
DMA works by applying an oscillating force to the material and the resultant
displacement of the sample is measured. From this, the stiffness can be
determined and the modulus and tan δ can be calculated. Tan δ is the
ratio of the loss modulus to the storage modulus. By measuring the phase
lag in the displacement compared to the applied force it is possible to
determine the damping properties of the material. Tan δ is plotted against
temperature and glass transition is normally observed as a peak since the
material will absorb energy as it passes through the glass transition.
Thermal Analysis
Quantitation of
the Amorphicity
of Lactose Using
Material Pockets

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WHITE
PAPER
Implementation of USP New Chapters <232> and <233>
on Elemental Impurities in Pharmaceutical Products
Introduction
For more than 100 years, the standard method for measuring
elemental impurities in pharmaceutical products sold in the
United States has been the “Heavy Metals Test,” described
in Chapter 231 of the United States Pharmacopeia’s (USP)
National Formulary (NF).1
This test is based on a sulfide
precipitation of the analyte elements with a thioacetamide
(C2H5NS) solution, and assumes that all analytes behave in
a similar manner to a lead standard with which samples are
compared. When the USP heavy metals method was first
published, it was only intended as a screening tool with results
being reported as < 10 ppm Pb. Additionally, although USP
Chapter <231> is listed as a “Heavy Metals Test,” it was
initially intended to detect a larger group of elements like Pb,
Hg, Bi, As, Sb, Sn, Cd, Ag, Cu, Mo, and Se, but there was no
clear definition of which individual elements the method was
expected to detect.
One of the many limitations of this approach is the assumption
that the reaction mechanism for the formation of the sulfides
in the sample is very similar to the formation of lead sulfide
in the standard solution and is not impacted significantly by
the sample matrix. However, since many metals’ sulfides can
form colloids, which behave very differently to solutions, the
method requires that the visual comparison is performed in a
relatively short period of time (< 5 mins.) after the precipitate
has formed but before the sample starts to become unstable.
The problem is that different analysts can differ in their
interpretation of a result by how they perform the visual
comparison, and it is fairly typical that inexperienced analysts
may not understand the subtleties of how to accurately and
consistently read the sample and standard solutions each time.
Another limitation of the technique is that ~ 2 g of sample is
required in order to achieve the desired detection capability.
Such a large sample weight is often difficult to acquire at
the early stages of drug development due to the very limited
supply. This is additionally compounded by the sample
preparation procedure, involving ashing at 600 °C and acid
dissolution of the sample residue, which is notoriously prone
to sample losses. In fact, some studies have shown that up
to 50% of the metals may be lost during the ashing process,
particularly the volatile elements like selenium (Se) and
mercury (Hg). The loss of metals is also matrix-dependent,
and because the procedures are time-consuming and
labor-intensive, recoveries can vary significantly among
differing analysts.
Expert Committee Findings
The general consensus by a panel of experts in a 2008
workshop organized by the Institute of Medicine (IOM) was that
the current methodology for metals testing was inadequate
and should be replaced by instrumental methods of greater
specificity and sensitivity for a wide range of metals of interest.
The challenge, however, was finding a suitable analytical
method and combining it with risk assessment studies to get a
better understanding of what metals have a negative impact on
public health. Due to known toxicity effects and the potential
for contamination in pharmaceutical ingredients, there was
agreement that lead (Pb), mercury (Hg), arsenic (As), and
cadmium (Cd) would need to be measured at toxicologically-
relevant concentrations. In addition, metal catalysts such as
the platinum group metals (PGMs) – platinum (Pt), palladium
(Pd), ruthenium (Ru), rhodium (Rh), and rubidium (Rb) – used
in the production of many pharmaceuticals, should be included
based on the likelihood of them being present. Also, a wider
range of metals used as organometallic reagents were used
in the manufacturing process and therefore at risk of being
present. An important consideration was the form of the metal,
particularly with arsenic and mercury. For example, dietary
Author
PerkinElmer, Inc.
Shelton, CT
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PerkinElmer, Inc.
940 Winter Street
P: (800) 762-4000 or
(+1) 203-925-4602
www.perkinelmer.com
Copyright ©2013, PerkinElmer, Inc.All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc.All other trademarks are the property of their respective owners.
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