VOLUME 10

SPOTLIGHTON APPLICATIONS.FOR A BETTERTOMORROW.

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PerkinElmer

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INTRODUCTION

PerkinElmer Spotlight on Applications e-Zine – Volume 10

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.

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PerkinElmer

CONTENTS

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Consumer Products• Analysis of Consumer Products by Headspace Trap GC/MS using the Clarus SQ 8

• A Spectroscopic In Vitro Method for the Calculation of Sunscreen SPF Values

Energy & Industrial• ICP-OES Analysis of FeCr Alloys Prepared by Sodium Peroxide Fusion

• Differential Scanning Calorimetry Performance Comparison

• The Determination of C1 to C5 Hydrocarbons in Gas Streams Using the PerkinElmer Swafer Technology

• Analysis of Wear Metals and Additive Package Elements in New and Used Oil Using the Optima 8300 ICP-OES with Flat Plate Plasma Technology

Environmental• Driving Productivity and Increasing the Speed of Analysis

• Determination of As, Se and Hg in Waters by Hydride Generation/Cold Vapor Atomic Absorption Spectroscopy

Food & Beverage• Toxic Trace Metals in Edible Oils by Graphite Furnace Atomic Absorption Spectrophotometry

• The Qualitative Characterization of Fruit Juice Flavor using a TurboMatrix HS Trap and a Clarus SQ 8 GC/MS

• Analysis of Pb, Cd and As in Tea Leaves Using Graphite Furnace Atomic Absorption Spectrophotometry

• Quantification of Essential Metals in Spice Mixtures for Regulatory Compliance Using the Flame Atomic Absorption Spectrophotometry

Pharmaceuticals & Nutraceuticals• Analysis of Ginsenosides in Ginseng Root with the PerkinElmer Flexar FX-15 System

Equipped with a PDA Detector

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

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Fragrant soaps and detergents are a ubiquitous part of our modern society and add a certain romance to what would otherwise be mundane household chores. Great care and expense is spent in formulating the exact mixture of fragrant organic compounds to differentiate “apple blossom” or “crisp apple” from simple “apple” scent. At the other end

of the spectrum are “fragrance-free” products – products that contain no fragrance producing organics, natural or otherwise. Unfortunately the term “fragrance-free” is unregulated and the actual composition of these products is left to the manufacturer’s discretion. For both situations a comprehensive analytical technique is necessary to measure both composition and quality of any volatile organic compounds present. In this application brief we describe a quick and simple analytical technique using headspace trap gas chromatography/mass spectrometry (GC/MS) to determine the volatile fragrance compounds contained in various consumer products.

Gas Chromatography/ Mass Spectrometry

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

Author

Ruben Garnica

Andrew Tipler

PerkinElmer, Inc. Shelton, CT 06484 USA

Analysis of Consumer Products by Headspace Trap GC/MS using the Clarus SQ 8

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A Spectroscopic In Vitro Method for the Calculation of Sunscreen SPF Values

Introduction

The sun produces ultraviolet (UV) A and ultraviolet B rays that reach the Earth, which are part of an elec-tromagnetic spectrum. UVA ray wavelengths range from 400 nanometers to 320 nanometers, while UVB rays range from 320 nanometers to 290 nanometers. UVA can penetrate both the upper layer of skin, the epidermis, as well as the lower layer of skin, the dermis. It is most often responsible for damaging

keratinocytes in the epidermis, where skin cancer is typically found. UVB, although it does not penetrate the dermis, is more intense because of it’s shorter wavelengths. However, both can be extremely harmful to humans, as they can cause sunburns, skin cancer, and other skin damage. In order to prevent these problems from happening, sunscreen use is recommended. Sunscreen protects skin by either absorbing or reflecting the harmful ultraviolet rays, preventing them from reaching the skin. Using sunscreen while exposed to the sun can greatly reduce the chances of damaging skin cells and developing cancer. For this study the PerkinElmer® LAMBDA™ 1050 equipped with a 150 mm integrating sphere will be use to collect scatter transmission data for sunscreen placed on a tape substrate. Testing sunscreen on a tape model of human skin to calculate the SPF value is more convenient and economical than testing on human skin.

Author

Jillian F. Dlugos

Glenelg High School Glenelg, MD USA

PerkinElmer, Inc. Shelton, CT USA

CASE STUDY

Consumer Products

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Introduction

Ferroalloys, alloys of iron with sufficient amounts of one or more other elements present (V, Mo, Cr, etc.), are important as a source of various metallic elements in the production of all types of steels. They usually have low melting points and can be incorporated readily into molten steel where they provide a certain chemical composition with specified properties.1

The ferrochrome alloy is produced by electric arc melting of the mineral chromite (FeCr2O4). It is largely used for the production of stainless steels. Increasing the amount of chromium content in the steel allows for increased corrosion and oxidation resistance. Other alloying elements, such as nickel (Ni) or molybdenum (Mo), aid in making the steel more passive and increasing its stainless properties.2

The presence of unwanted impurities in the metal and slag may alter reaction temperatures and cause undesirable reactions of their own.1 The chemical analysis of the chromite ore and its final products are mandatory to assess the quality of the chromite ore and to optimize the grade of stainless steel production. Analysis of waste products is also needed to optimize recovery of chromium and other additives.2

ICP-Optical Emission Spectroscopy

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

Author

Chady Stephan

PerkinElmer, Inc.

Woodbridge, Ontario, Canada

ICP-OES Analysis of FeCr Alloys Prepared by Sodium Peroxide Fusion

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Introduction

Differential scanning calorimetry (DSC) is a commonly used technique for studying polymeric, pharmaceutical, and energetic materials. When considering which type of DSC to use to per-form a specified measurement one typically chooses either a Power Compensation, or Heat Flux design. These instruments are often referred to as double and single furnace DSC respec-tively. PerkinElmer is the only vendor to provide both designs to customers, because we believe that both technologies provide

unique advantages and users can choose the best type of DSC to meet their specific need. One of the more common questions is how do the instruments data compare when perform-ing a standard measurement? To answer this question, a standard polystyrene (PS) and low-density polyethylene (PE) sample are tested using the conventional heat-cool-reheat method.

DSC 8000/8500

• PerkinElmer’snewflagshipDSC8000andDSC8500wasdevelopedfortheuser’sneedfor greater sensitivity and accuracy. They can be used for many applications including QA/QC applications, studying processes in plastics and pharmaceuticals.

• TheDSC8000providesoutstandingsensitivityandreproducibility.ItfeaturesPerkinElmer’sproprietary double-furnace technology, which directly measures the heat flow between twoindependentfurnaces.Itprovidesthemostpreciseenergymeasurementsoverthewhole temperature range of any DSC in order to meet the most demanding applications. Thereisanoptional96-positionautosampleravailableandtheDSC8000canbeupgradedtoaDSC8500.

• TheDSC8500,whileprovidingallofthefeaturesoftheDSC8000,alsooffersHyperDSC® heating and cooling with extremely fast controlled scanning rates and in-situ ballistic cooling important for applications such as isothermal crystallization, polymorph/amorphous-material studies and high sensitivity measurements.

Differential Scanning Calorimetry Performance Comparison

Thermal Analysis

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

Author

Justin Lang Ph.D.

PerkinElmer, Inc. 710 Bridgeport Avenue Shelton, CT 06484

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Introduction

The determination of light hydrocarbons in refinery and other gases is typically performed through the use of packed columns and mechanical rotary valves. For example ASTM® Method D-2597 adopts this approach. A gas sampling valve delivers a small metered quantity of the sample gas into a non-polar packed column. The C1 to C5 hydrocarbons are allowed to elute from this column and into a second packed column with a polar stationary phase. At that point

a rotary valve is actuated to reverse the flow of carrier gas through the precolumn and backflush any residual sample in that column to a detector to determine the total C6+ content in the sample. In the meantime, chromatography of the C1 to C5 content proceeds on the second column for separation, identification and quantification. The whole analysis takes about 20 minutes and getting acceptable chromatographic separation is often a challenge because of normal variations in the columns.

In this application note, a new method is described for this analysis that uses a Swafer™ backflushing technology with capillary columns under isothermal conditions to both improve the chromatographic separation and to reduce the analysis cycle time to just over 5 minutes.

Experimental

For this analysis, an S-Swafer is used to manage the backflushing operations on the precolumn rather than a more conventional mechanical valve. The S-Swafer uses the Deans pressure balanced technique to reverse gas pressures across a GC column to initiate the backflushing process. Such systems have been widely used for 50 years – particularly for capillary columns where low thermal mass, inertness and low dead volumes are critical.

Gas Chromatography

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

Author:

A. Tipler

PerkinElmer, Inc. Shelton, CT 06484 USA

The Determination of C1 to C5 Hydrocarbons in Gas Streams Using the PerkinElmer Swafer Technology

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Introduction

The analysis of new and used oil for concentration trends of wear metals and for formulation or depletion of additive package metals has been around for over 30 years. Wear metals such as copper (Cu) and iron (Fe) may indicate wear in an engine or any oil-wetted compartment. Boron (B), silicon (Si) or sodium (Na) may indicate contamination from dirt or antifreeze leading to a failure. Additive elements such as calcium (Ca), phosphorus (P) and zinc (Zn) are analyzed for depletion which contributes to wear since these elements contribute to certain key lubri-cation characteristics. A sound maintenance program, which routinely measures metals in the lubricating oils, not only

reduces the expense of routinely dismantling the components for visual inspection, but can indicate unexpected wear before component failure.

Atomic absorption spectrometers (AAS) were first used for these applications in the early-to-mid 1960s. As the number of elements and samples grew over the years, inductively coupled plasma-optical emission spectrometers (ICP-OES) were used for oil analysis. Today, many oil analysis labs will handle between 500 to 2000 samples per day and analyze from 15 to 24 elements per sample.

Many improvements to ICP technology have taken place over the years with the most recent being the replacement of the helical load coil used to generate the plasma. The Optima™ 8x00 ICP-OES series (Figure 1 – Page 2) utilizes the new Flat Plate™ plasma technology that replaces the traditional helical coil design used since the inception of the inductively coupled plasma. The Flat Plate plasma technology utilizes two flat induction plates

ICP-Optical Emission Spectroscopy

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

Author

David Hilligoss

PerkinElmer, Inc. Shelton, CT USA

Analysis of Wear Metals and Additive Package Elements in New and Used Oil Using the Optima 8300 ICP-OES with Flat Plate Plasma Technology

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Case study Environmental

Driving Productivity and Increasing the Speed of Analysis

South West Water is responsible for maintaining and monitoring the quality of drinking and bathing waters and the sewage

system network in a region of England. They do this effectively through a central analytical facility. In early 2010, as part of the rolling replacement programme, the ICP-MS instrument was identified as due for renewal. The analytical team were looking for an instrument that could be relied upon to have minimum downtime and be a workhorse for high sample throughput; but also offer flexibility to adapt to changing business requirements and complete investigative work if required. After the evaluation of the top three suppliers, the NexION® 300 ICP-MS from PerkinElmer was selected. The flexibility offered by NexION having both a collision and dynamic reaction cell ensures that the lab is future proofed. Being fully prepared to handle any changes in sample matrices and still benefit from sensitive, reproducible results day in day out.

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Introduction

Contamination of industrial and municipal water supplies with arsenic (As), selenium (Se), and mercury (Hg) can occur from natural deposits, industrial discharge, runoff from mining, landfill and agricultural operations. Consumption of contaminated water can cause skin damage (As), kidney and nervous system damage (Hg) and numbness in the fingers and toes (Se).1 The U.S. Environmental Protection Agency (EPA) and the Canadian Council of Ministers of the Environment (CCME) have guidelines on the concen-tration of As, Se and Hg for the protection of marine

and freshwater aquatic life and the protection of agriculture.1,2 Due to the low levels of these guidelines for As, Se, and Hg, it is important to have analytical measurements that are precise and accurate with low amounts of noise.

Hydride generation (HG) is a very effective analytical technique developed to separate hydride forming metals, such as Se and As, from a range of matrices and varying acid concentrations. The heated quartz tube atomizer is particularly useful for the determination of arsenic and selenium because the absorption wavelengths for these elements are below 200 nm in an area subject to intense interference from flame radicals that can significantly affect detection limits. Mercury can be easily reduced in solution to generate elemental mercury, otherwise known as cold vapor (CV). This technique is also effective at separating mercury from a range of matrices. These analytical techniques can improve detection limits by a factor of approximately 3000 times that of flame detection limits and typically have less interference than graphite furnace techniques.

Atomic Absorption

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

Author

Aaron Hineman

PerkinElmer, Inc. Ontario, Canada

Determination of As, Se and Hg in Waters by Hydride Generation/ Cold Vapor Atomic Absorption Spectroscopy

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Introduction

Graphite furnace atomic absorption spectropho-tometry (GFAAS) has been widely applied to the determination of trace elements in food due to its selectivity, simplicity, high sensitivity, and its capability for accurate determinations in a wide variety of matrices. Edible oils are generally low in trace element concentrations, however, metals such as arsenic (As), lead (Pb), cadmium (Cd), chromium (Cr), and selenium (Se) can be found and are known for their toxicities which affect the health of consumers. The determination

of toxic elements from naturally occurring or production-contamination sources in oils can be determined by using GFAAS or inductively coupled plasma mass spectrometry (ICP-MS). When only a few elements are being analyzed, GFAAS is the preferred choice. It is easy to learn, faster in setting up, and simpler to use than ICP-MS. GFAAS is also lower in initial capital investment and has a lower operating and maintenance cost. Sample pretreatment procedures for edible oils are normally required prior to instrumental analysis in order to eliminate the organic matrix. Wet, dry or microwave digestion, dilution with organic solvent, and extraction methods can be time consuming and require more operator training than a direct analysis method.

Atomic Absorption

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

Authors

Surasak Manarattanasuwan Senior Inorganic Product Specialist

PerkinElmer, Inc. Thailand

Toxic Trace Metals in Edible Oils by Graphite Furnace Atomic Absorption Spectrophotometry

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Introduction

The PerkinElmer® TurboMatrix™ Headspace Trap system coupled with a Clarus® SQ 8 GC/MS is a very convenient means of identifying low concentration volatile organic compounds (VOCs) in foodstuffs. In this application note, the VOCs in various fruit juices were investigated. Sample preparation simply involved dispensing a fixed volume of fruit juice into a sample vial and sealing it. The analysis was fully automated.

Gas Chromatography/ Mass Spectrometry

A P P L I C A T I O N N O T E

Author

A. Tipler, Senior Scientist

PerkinElmer, Inc. Shelton, CT 06484 USA

The Qualitative Characterization of Fruit Juice Flavor using a TurboMatrix HS Trap and a Clarus SQ 8 GC/MS

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Introduction

Tea is drunk by about half of the world’s population. It is widely cultivated and consumed in Southeast Asia. Tea is rich in many trace inorganic elements.1,2 In addition to many essential elements required for human health, some toxic elements may also be present in tea leaves. This could be due to polluted soil,

application of pesticides, fertilizers or industrial activities. There is often little information available about the safety of tea leaves and finished tea products with respect to heavy metal contamination. Due to the significant amount of tea consumed, it is important to know the toxic metal contents.

The toxicity and effect of trace heavy metals on human health and the environment has attracted considerable attention and concern in recent years. Among the heavy metals, lead (Pb), cadmium (Cd) and arsenic (As) are especially toxic and are harmful to humans even at low concentrations. They have an inherent toxicity with a tendency to accumulate in the food chain and a particularly low removal rate through excretion.3 Exposure to heavy metals above the permissible level can cause high blood pressure, fatigue, as well as kidney and neurological disorders. Heavy metals are also known to cause harmful reproductive effects.4

A major challenge in the analysis of tea leaves is the extremely low analyte levels and the very high matrix levels. For many years, graphite furnace atomic absorption spectrophotometry (GFAAS) has been a reliable technique and the preferred method for this analysis. The use of longitudinal Zeeman background correction and matrix modifiers help to achieve extremely low detection limits in high matrix samples such as tea leaves, making GFAAS an indispensible tool for carrying out such analyses.

Atomic Absorption

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

Author

Praveen Sarojam, Ph.D.

PerkinElmer, Inc. Shelton, CT 06484 USA

Analysis of Pb, Cd and As in Tea Leaves Using Graphite Furnace Atomic Absorption Spectrophotometry

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Introduction

Foods, together with water, provide the major proportion of the total daily intake of trace elements by humans. Spices and vegetables are some of the most common foods in the human diet around the world. Besides polluted soil and water, foods can also be contaminated with trace metals by the introduction of mechanized farming, the increasing use of chemicals, food processing and packaging, etc. In order to minimize adverse impact, it is important to measure and continuously monitor the levels of trace elements in various kinds of food materials. Trace element food composition data are also important for both consumers and health professionals. In recent years, food labeling legislation has enforced this requirement. Trace element determination in complex matrices, such as food, often requires sample preparation prior to determination by instrumental techniques.1

Cobalt (Co), copper (Cu), manganese (Mn), nickel (Ni) and zinc (Zn) are all essential elements, not only for mammals, but also for plants. They play important roles in many biological processes including carbohydrate and lipid metabolism.2 For example, a daily copper intake of 1.5 - 2.0 mg is essential and copper at nearly 40 ng/mL is required for normal metabolism of many living organisms.3 However, copper at higher levels is toxic to the circulatory system and kidneys. The trace element content of food items for all the essential elements mentioned above must be controlled on a daily basis.

Atomic Absorption

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

Author

Praveen Sarojam, Ph.D.

PerkinElmer, Inc. Shelton, CT 06484 USA

Quantification of Essential Metals in Spice Mixtures for Regulatory Compliance Using Flame Atomic Absorption Spectrophotometry

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Introduction

The root of the panax genus plant (also called Ginseng) has been used as an herbal medicine in Asia for over two thousand years for its purported various health benefits, including (but not limited to), antioxidant, anticarcinogenic, anti- inflammatory, antihypertensive and anti-diabetic. The pharmacologically active compounds behind the claims of ginseng’s efficacy are ginsenosides; their underlying mechanism of action although

not entirely elucidated appears to be similar to that of steroid hormones. There are a number of ginseng species, and each has its own set of ginsenosides. In fact, more than forty different ginsenosides have been identified. Ginsenosides are a diverse group of steroidal saponins with a four ring-like steroid structure with sugar moieties (Figure 1); they are found exclusively in ginseng plants and are in higher concentration in their roots. There are two main groups of ginsen-osides: the panaxadiol group or Rb1 group that includes Rb1, Rb2, Rc, Rd, Rg3, Rh2, and Rh3; and the panaxatriol group or Rg1 group that includes Rg1, Re, Rf, Rg2 and Rh1.

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

Analysis of Ginsenosides in Ginseng Root with the PerkinElmer Flexar FX-15 System Equipped with a PDA Detector

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Introduction

Acetaminophen and aspirin are the drugs of choice used to relieve the symptoms of common headache. Acetaminophen, which is also called paracetamol, is widely used as a pain reliever (analgesic) and fever reducer (antipyretic). Because of its fast onset (eleven minutes after intake), acetaminophen is very effective. However, every year its misuse (dose exceeding the daily adult limit of four grams) can cause fatal liver damage. In fact, acetaminophen

toxicity is the main cause of acute liver failure and accounts for most drug over-doses in the United States. The other common active ingredient in headache medicines is acetylsalicylic acid (aspirin), which is an analgesic, antipyretic and anti-inflammatory drug. Despite its usefulness, aspirin has a harmful side effect. For many people it can cause or exacerbate gastrointestinal ulcers by destroying the mucosal lining. This is a major setback for a medicine that is otherwise very inexpensive and can also be used for its antiplatelet effect to prevent heart attack and stroke. In formulations specially designed to treat common headaches (tension headache), acetaminophen and aspirin are often combined with caffeine. In these formulations, caffeine not only increases the effectiveness of the two drugs but it also stimulates the central nervous system and temporarily wards off tiredness.

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

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

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