VOLUME 11

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

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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 page within the e-zine.

We invite you to explore, enjoy and learn!

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PerkinElmer

CONTENTS

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Energy & Industrial• Improved HyperDSC Method to Determine Specific Heat Capacity of Nanocomposites and

Probe for High-Temperature Devitrification

• Polymer Identification Using Mid Infrared Spectroscopy

• An Introduction to Flow Field Flow Fractionation and Coupling to ICP-MS

• Coupling Flow Field Flow Fractionation to ICP-MS for the Detection and Characterization of Silver Nanoparticles

Environmental• The Determination of Low Levels of Benzene, Toluene, Ethyl Benzene and Xylenes (BTEX) in

Drinking Water by Headspace Trap GC/MS

• Improved Sensitivity and Dynamic Range Using the Clarus SQ 8 GC/MS System for EPA Method 8270D Semi-Volatile Organic Compound Analysis

Food & Beverage• Qualifying Mustard Flavor by Headspace Trap GC/MS using the Clarus SQ 8

• Simultaneous Analysis of Nine Food Additives with the PerkinElmer Flexar FX-15 System Equipped with a PDA Detector

• Analysis of Pb, Cd and As in Spice Mixtures Using Graphite Furnace Atomic Absorption Spectrophotometry

• Practical Food Applications of Differential Scanning Calorimetry (DSC)

Forensics & Toxicology• Opiates in Urine by SAMHSA GC/MS

• Characterization of Single Fibers for Forensic Applications Using High Speed DSC

Pharmaceuticals & Nutraceuticals• Analysis of Drug Substances in Common Cold Medicines with the PerkinElmer

Flexar FX-15 System Equipped with a PDA Detector

• Detection and Quantification of Formaldehyde by Derivatization with Pentafluorobenzylhydroxyl Amine in Pharmaceutical Excipients by Static Headspace GC/MS

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Introduction

There has been tremendous interest in recent years in nanocomposites – using small scale particulate fillers – to improve the properties of thermoplastics and thermosets. For example, the effect of using such small scale filler particles is such as to toughen the plastics, reduce vapor transfer, and improve transparency. One rapid way to quantify the effect 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.

Differential Scanning Calorimetry

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

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 Method to Determine Specific Heat Capacity of Nanocomposites and Probe for High-Temperature Devitrification

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Introduction

Synthetic polymers are very widely used today, with diverse applications in various industries such as food, automotive, and 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.

Infrared Spectroscopy

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Polymer Identification Using Mid Infrared Spectroscopy

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Whitepaper Inductively Coupled Plasma – Mass Spectrometry

AuthorsDenise 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

Introduction

Inductively coupled plasma-mass spectrometry (ICP-MS) is the method of choice for analysis of most elements across the periodic chart. 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.

An Introduction to Flow Field Flow Fractionation and Coupling to ICP-MS

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Introduction

Analysis of nanomaterials should include characterization of composition as well as size. Many techniques are capable of sizing nano-size particles, such as dynamic light scattering (DLS), UV/Vis spectrophotometry, and transmission electron microscopy (TEM), yet provide no information on the composition of the particle and/or are time intensive and costly. Inductively coupled plasma-mass spectrometry (ICP-MS), however, is a standard instrument in many analytical laboratories 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.

ICP-Mass Spectrometry

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

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 Flow Fractionation to ICP-MS for the Detection and Characterization of Silver Nanoparticles

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Introduction

BTEX is a grouping of structurally similar volatile organic compounds including benzene, toluene, ethyl benzene and the three xylene isomers. These compounds are known pollutants and are typically found near petroleum production and storage sites. BTEX are regulated toxic compounds while benzene is also an EPA target carcinogen. The investigation of 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.

Gas Chromatography/ Mass Spectrometry

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Author

Lee Marotta

PerkinElmer, Inc. Shelton, CT 06484 USA

The Determination of Low Level Benzene, Toluene, Ethyl Benzene, and Xylenes (BTEX) in Drinking Water by Headspace Trap GC/MS

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Introduction

U.S. Environmental Protection Agency (EPA) Method 8270D – Semi-Volatile Organic Compounds by Gas Chromatography/Mass Spectrometry (GC/MS) – is a common and wide ranging method employed in nearly all commercial environmental laboratories. The analysis focuses on the detection of trace level semi-volatile organic compounds in extracts from solid waste matrices, soils, air sampling media and water samples. 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.

Gas Chromatography/ Mass Spectrometry

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Authors

Yury Kaplan

Ruben Garnica

PerkinElmer, Inc. Shelton, CT 06484 USA

Improved Sensitivity and Dynamic Range Using the Clarus SQ 8 GC/MS System for EPA Method 8270D Semi-Volatile Organic Compound Analysis

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Mustard is a common condiment used across many cultures and culinary styles to enhance the dining experience. It is derived from the mustard seed and is used either as a dried spice, spread or paste when the dried spice is mixed with water, vinegar or other liquid. The characteristic sharp taste of mustard arises from the isothiocyanates (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.

Gas Chromatography/ Mass Spectrometry

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Author

Ruben Garnica

Andrew Tipler

PerkinElmer, Inc. Shelton, CT 06484 USA

Qualifying Mustard Flavor by Headspace Trap GC/MS using the Clarus SQ 8

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Introduction

Food additives are natural or synthetic substances that are added in food, beverage and pharmaceutical products for their microbicidal, preservative and flavoring properties. Among the commonly used additives, benzoic acid and its salts are widely used in beverage and food 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.

UHPLC

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

Author

Njies Pedjie

PerkinElmer, Inc. Shelton, CT 06484 USA

Simultaneous Analysis of Nine Food Additives with the PerkinElmer Flexar FX-15 System Equipped with a PDA Detector

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Introduction

The toxicity and effect of trace heavy metals on human health and the environment has attracted considerable attention and concern in recent years. With an inherent toxicity, a tendency to accumulate in the food chain and a particularly low removal rate through excretion,1 lead (Pb), cadmium (Cd) and arsenic (As) cause harm to humans even at low 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

Atomic Absorption

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Author

Praveen Sarojam, Ph.D.

PerkinElmer, Inc. Shelton, CT 06484 USA

Analysis of Pb, Cd and As in Spice Mixtures using Graphite Furnace Atomic Absorption Spectrophotometry

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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 R&D purposes. DSC applications are used from troubleshooting up to new product developments.

Differential Scanning Calorimetry

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Authors

Patricia Heussen

Unilever Research & Development Vlaardingen, The Netherlands

Peng Ye, Kevin Menard, Patrick Courtney

PerkinElmer, Inc. Shelton, CT 06484 USA

Practical Food Applications of Differential Scanning Calorimetry (DSC)

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Introduction

The United States Department of Health and Human Services (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.

Gas Chromatography/ Mass Spectrometry

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

Author

Timothy D. Ruppel

PerkinElmer, Inc. Shelton, CT 06484 USA

Opiates in Urine by SAMHSA GC/MS

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Introduction

Crime or forensic laboratories must frequently work with very small samples in order to determine the type of material and its possible manufacturer for investigatory and evidence purposes. An example would be in the characterization of single fibers found at the crime scene. Fibers are useful for forensic purposes, as they tend to cling 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

Differential Scanning Calorimetry

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Characterization of Single Fibers for Forensic Applications Using High Speed DSC

DSC 8500

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Introduction

The common cold is a frequent upper respiratory tract infection caused by a number of different types of viruses. Common cold affects billions of 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.

UHPLC

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Author

Njies Pedjie

PerkinElmer, Inc. Shelton, CT USA

Analysis of Drug Substances in Common Cold Medicines with the PerkinElmer Flexar FX-15 System Equipped with a PDA Detector

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Introduction

Although considered pharmacologically inert, pharmaceutical excipients have been shown to interact with active drug sub-stances to affect the safety and efficacy of drug products.1 Therefore, there is an 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 degradation of several drug products where it can form adducts with primary and/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.

Gas Chromatography/ Mass Spectrometry

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Detection and Quantification of Formaldehyde by Derivatization with Pentafluorobenzylhydroxyl Amine in Pharmaceutical Excipients by Static Headspace GC/MS

Figure 1. Structure and properties of formaldehyde.

Author

Padmaja Prabhu

PerkinElmer, Inc. Shelton, CT USA

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By Industry:

• Consumer Products• Energy• Environmental• Food, Beverage & Nutraceuticals• Forensics• Lubricants• Pharmaceutical Development & Manufacturing• Polymers/Plastics• Semiconductor & Electronics

By Technology:

• 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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