PerkinElmer Spotlight on Analytical Applications e-Zine – Volume 15


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Spotlight on Applications is a quarterly compendium of recent applications, delivering a variety of topics that address the pressing issues and analytical challenges you may face today. Our e-zine covers a broad range of applications within various industries – all accessible online at your convenience.

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  2. 2. PerkinElmerTABLEOFCONTENTSINTRODUCTIONPerkinElmer Spotlight on Applications e-Zine – Volume 15PerkinElmer knows that the right training, methods and application support areas integral to getting answers as the instrumentation. That’s why PerkinElmer hasdeveloped a novel approach to meet the challenges that today’s labs face, deliveringyou complete solutions for your application challenges.We are pleased to share with you our Spotlight on Applications e-zine, whichdelivers a variety of topics that address the pressing issues and analytical challengesyou may face in your application areas today.Our Spotlight on Applications e-zine consists of a broad range of applications you’ll beable to access at your convenience. Each application in the table of contents includesan embedded link which takes you directly to the appropriate page within the e-zine.We invite you to explore, enjoy and learn!Be sure to receive futureissues by subscribing here.
  3. 3. PerkinElmerCONTENTSTABLEOFCONTENTSEnvironmental• Speciation of Organotin Compounds in Biological Tissues by GC/ICP-MS• Benefits of the NexION 300 ICP-MS Coupled with a seaFAST 3 Sampling System for theAutomated, High-Throughput Analysis of Seawater SamplesConsumer Products• Analyzing Parabens in Lipstick using DSA-TOF• The Chemical Analysis of Bisphenol A in PlasticFood Beverage• Safeguarding Food from Pesticides by UHPLC After Extraction with the QuEChERS Method• Rapid Detection of Vanilla Bean Extract Adulteration with Tonka Bean Extract withNo Chromatography or Sample Preparation• Targeted Screening of 130 Pesticides in QuEChERS Extracts of Lettuce LeavesUsing UHPLC-TOF and High Throughput Screening Software• Rapid Screening of Adulteration in Pomegranate Juice with Apple Juice Using DSA/TOFwith Minimal Sample PreparationPharmaceuticals Nutraceuticals• Identification of Impurities Using Accurate Mass, Sensitivity and Wide DynamicRange of the AxION 2 TOF MS• The Application of Mesh Material Pockets in DMA Analysis of Amorphous andCrystalline Lactose PowdersForensics and Toxicology• Automated Direct Sample Analysis (DSA/TOF) for the Rapid Screening and Confirmationof Illicit Street Drugs• The Detection of Ethyl Centralite using DSA-TOF
  4. 4. TABLEOFCONTENTSTOF MSDirect Sample analySiSEasy to useNo chromatographyProtects consumers• DSA/TOF direct analysis of lipstick in a glass capillary confirms presence of parabens with accurate mass• Analysis was performed in 15 seconds with no sample preparation and external calibration• Parabens are widely used in lipsticks to improve shelf life but links to breast tumours have been found.Chemical: Parabens in LipstickFor a complete listing of our global offices, visit ©2012, perkinelmer, inc. all rights reserved. perkinelmer®is a registered trademark of perkinelmer, inc. all other trademarks are the property of their respective owners.010590_01PerkinElmer, Inc.940 Winter StreetWaltham, ma 02451 USap: (800) 762-4000 or(+1) 203-925-4602www.perkinelmer.comDownload Application Brief
  5. 5. Download Application BriefTABLEOFCONTENTSFor a complete listing of our global offices, visit ©2013, PerkinElmer, Inc. All rights reserved. PerkinElmer®is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners.010858_01PerkinElmer, Inc.940 Winter StreetWaltham, MA 02451 USAP: (800) 762-4000 or(+1) 203-925-4602www.perkinelmer.comTOF MSDIrECt SAMPlE AnAlySISChemical: Bisphenol A in PlasticEasy-to-useNo sample prep orchromatographyProtects consumers• DSA/TOF direct analysis of a section of plastic bottle confirms presence of BPA with accurate mass.• The analysis was performed in 30 seconds with no sample preparation and external calibration.• Bisphenol A (BPA) is used along with other materials to make plastics. It is characterized as an endocrine disruptor mimicking natural hormones which has elevated safety concerns about it leaching into our food from the packaging and negatively impacting human health.• In 2010, the FDA warned of the possible hazard to young children and BPA was banned from baby bottles.
  6. 6. Download Entire Application NoteTABLEOFCONTENTSGC/ICP-MSa p p l i c a t i o n n o t eAuthors:Joaudimir Castro, Emmanuel Tessier,Kenneth Neubauer* and OlivierF.X. DonardLaboratoire de Chimie AnalytiqueBio-inorganique et EnvironnementIPREM UMR 5254 CNRSUniversité de Pau et des Pays de l’Adour,Hélioparc, 64053 Pau, France*PerkinElmer, Inc.710 Bridgeport AvenueShelton, CTIntroductionThe environmental concerns regardingorganotin compounds are of greatimportance due to their extensive usefor agricultural, industrial and domestic applications.1Butyl- and phenyl-tinshave been widely used as active biocides in applications such as antifoulingpaints, PVC stabilizers, timber treatment, and others.2For example, the useof antifouling paints resulted in extensive damage to non-target organismsat ultratrace concentration levels (ppt) and accumulation in sediments andbiota.3-4As a result, the European Union (EU) added tributyl tin (TBT) and itsdegradation products to the list of priority pollutants (Decision 2455/2001/ECamending the Water Framework Directive 2000/60/EC).4The U.S. EnvironmentalProtection Agency (EPA) established the ambient aquatic-life water qualitycriteria for TBT in which the criterion to protect marine aquatic life fromchronic toxic effects is 3 ng Sn/L and from acute toxic effects 172 ng Sn/L.4Thedifferent toxicity levels between TBT, triphenyl tin (TPhT) and their degradationproducts (di- and monosubstituted and inorganic tin,) as well as the monitoringof their environmental impact, makes organotin speciation analysis necessary.5Nowadays, the method of choice for trace organometals analysis is gaschromatography coupled with inductively coupled plasma mass spectrometry(GC/ICP-MS) due to its high sensitivity, selectivity, multielementaland multiisotopic capabilities.3To carry out organotin speciation viaGC/ICP-MS, a derivatization reaction with sodium tetrapropylborate orsodium tetraethylborate is necessary to increase the volatility of the species.In addition, for the analysis of complex matrices, such as biological tissuesSpeciation of OrganotinCompounds in BiologicalTissues by GC/ICP-MSGC/ICP-MS
  7. 7. TABLEOFCONTENTSDownload Entire Application NoteIntroductionThe determination of trace elementsin seawater presents unique challengesfor ICP-MS that are rarely encounteredwith any other type of sample. The highconcentrations of matrix components,such as sodium, magnesium andchloride ions, create polyatomic spectralinterferences that make the determinationof elements, such as arsenic (As),chromium (Cr), vanadium (V), iron (Fe) andselenium (Se), very challenging. Even forelements like cadmium (Cd), thallium(Tl) and lead (Pb), where spectral interferences are less problematic, low-pptconcentrations in open-ocean seawater are very difficult to determine with goodaccuracy and precision. Dilution has often been used to cope with high matrixsamples, but it is not a realistic option for many transition metals whenultra-trace detection limits are required. Additionally, routine aspiration of seawater,even with some dilution, causes deposits to form around the sampler andskimmer cone orifices. In some ICP-MS systems, deposits can reach the ionoptics and cause long-term signal stability problems and frequent maintenanceand cleaning. However, the unique Triple Cone Interface and Quadrupole IonDeflector in the PerkinElmer®NexION®300 ICP-MS attenuate this problem.ICP-Mass Spectrometrya p p l i c a t i o n n o t eAuthorsEwa Pruszkowski, Ph.D.PerkinElmer, Inc.Shelton, CT USANathan Saetveit, Ph.D.Elemental ScientificOmaha, NE USABenefits of the NexION 300ICP-MS Coupled with aseaFAST 3 Sampling Systemfor the Automated,High-Throughput Analysisof Seawater Samples
  8. 8. TABLEOFCONTENTSIntroductionThe detection of pesticides in food matrices, suchas fruit and vegetables, requires an ever increasinguse of new technologies. Chromatographictechniques, both gas (GC) and liquid (LC), offera suitable means of addressing the analyticalrequirements. They enable screening to be carriedout rapidly both in gaseous and liquid phases – onsamples prepared using the “QuEChERS” (Quick,Easy, Cheap, Effective, Rugged, Safe) system, a fast and effective multi-residueextraction method.Employing UHPLC (Ultra High Performance Liquid Chromatography) with a PDA(Photo Diode Array) detector offers considerable advantages over standard LCanalysis. Indeed, it provides a very fast means of monitoring phytodrugs whichare permitted in concentrations of up to 10 μg/Kg. The use of a PDA detector,together with the development of a library of spectra, enables each substance tobe analyzed and identified correctly.Liquid Chromatographya p p l i c a t i o n n o t eAuthorsRoberto TroianoValentina ScanzaniPerkinElmer, Italia S.p.A.Monza, ItalySafeguarding Food fromPesticides by UHPLCAfter Extraction with theQuEChERS MethodDownload Entire Application Note
  9. 9. TABLEOFCONTENTSMass Spectrometrya p p l i c a t i o n n o t eAuthor:Avinash DalmiaPerkinElmer, Inc.Shelton, CT USAIntroductionVanilla is the second most expensivespice, and is widely used as a flavoringingredient in the food, beverage, cosmetic,pharmaceutical and tobacco industries.Pure vanilla bean extract is made bysoaking at least 13.35 ounces of vanillabeans in a gallon solution containing aminimum of 35% ethyl alcohol in water.The production of vanilla beans is quite expensive, since it is a very laborintensive process and harvesting takes place two to three years afterplanting. Due to this, the price of natural vanilla bean extract is quiteexpensive. It is quite often adulterated with cheaper tonka bean extract,which smells and tastes like vanilla bean extract due to the presence ofa compound called coumarin1. Since coumarin is absent in vanilla beanextracts, it can be used as a marker compound to detect its adulterationwith tonka bean extracts.Tonka bean extract is banned for human consumption by the FDA due toits adverse health effects caused by the presence of coumarin. Coumarinis banned in foods based on histological evidence of hepatoxicity inanimal experiments. Coumarin is toxic to the liver and kidneys and causesthinning of the blood. This is particularly dangerous for people takingblood thinning drugs because the interaction of coumarin and bloodthinners can increase the likelihood of bleeding2.Rapid Detection ofVanilla Bean ExtractAdulteration with TonkaBean Extract with NoChromatography orSample PreparationDownload Entire Application Note
  10. 10. TABLEOFCONTENTSIntroduction:The Food Quality protection Act (FQPA) in the United States (US)and the European Union (EU) directive 91/414/EEC require thatif pesticides are present in food they are below agreed levelsdue to the health risk posed by pesticides 1, 2. With the advent oflarge scale agricultural production, hundreds of pesticides havebeen synthesized in the last century and used widely to protectcrops. Newer pesticides continue to be synthesized for crop usagewhich makes it important to analyze both targeted (or expectedanalytes) and non-targeted pesticides in food and in the environment. Unlike a triplequadrupole instrument that only measures targeted analytes (defined by selected multiplereaction monitoring of analyte ions or MRMs), the time-of-flight (TOF) mass spectrometercan measure both targeted and non-targeted analytes3. TOF mass spectrometers collectfull spectrum information and hence the data can be re-examined for the presence ofthese “non-targeted” analytes. We present a study of pesticide analysis in a lettuceleaves extract that was obtained by the QuEChERS (Quick, Easy, Cheap, Effective,Rugged and Safe) method of food extraction. The lettuce extract was spiked with varyingconcentrations of a mix of 130 pesticides and analyzed by Ultra-High Pressure LiquidChromatography-Mass Spectrometry (UHPLC-MS) with a PerkinElmer AxION®2 TOF MSas the detector. We could detect the majority of the pesticides well within the EU limit ofdetection (LOD) requirement range of 10 ppb. The data was further analyzed using AxIONSoloTMhigh throughput software. The presence of each of the analytes when detectedabove the 10 ppb threshold was given a specific color code which helped to rapidlyscreen for presence/absence of all 130 analytes in each sample. A combination of shortrun times and powerful screening software helped simplify analysis and also reduce thetime of analysis.Liquid Chromatography/Mass Spectrometrya p p l i c a t i o n n o t eAuthors:Sharanya ReddyAriovaldo BisiPerkinElmer, Inc.Targeted Screening of 130Pesticides in QuEChERSExtracts of Lettuce LeavesUsing UHPLC-TOF andHigh ThroughputScreening SoftwareDownload Entire Application Note
  11. 11. TABLEOFCONTENTSIntroductionPomegranate juice is in high demand due to its well documentedhealth benefits. Studies based on a significant body of scientificresearch conducted on authentic pomegranate juice haveestablished that pomegranate juice has superior antioxidant activitycompared to other popular fruit juices such as grape, orange andapple1,2,3. These superior health benefits have led to a meteoric risein the popularity of pomegranate juice over the last 10 years. Thishas resulted in pomegranate juice having a significantly higher costthan other juices, especially in comparison to apple, orange and grape juice. This high costhas provided an economic incentive for the adulteration of pomegranate juice4. There are anumber of of other reasons for adulteration including: customers demanding their suppliersreduce costs; there comes a point when a supplier may adulterate the product to lower thecost and maintain a workable margin. Another reason for pomegranate juice adulteration isthat it is in high demand and short supply, leading to incentives to extend limited supplies bythe addition of other cheaper fruit juices.The adulteration of pomegranate juice is accomplished by using cheap ingredients. One ofthe common adulterants of pomegranate juice is a cheaper so called filler fruit juice such asapple juice. The advantage of adulterating pomegranate juice with apple juice is that it isclear and provides no noticeable change to the sugar content. Organic acid analysis plays afundamental role in testing the authenticity of pomegranate juice. One organic acid of interestis malic acid. Although it is present in both pomegranate and apple juice, the amount in applejuice is significantly higher than in pomegranate juice, 4.5 g/L and 0.57 g/L respectively5,6.Therefore, the adulteration of pomegranate juice with apple juice can be detected by theelevated levels of malic acid present in the juice. Analytical methods used routinely forMass Spectrometrya p p l i c a t i o n n o t eAuthor:Avinash DalmiaPerkinElmer, Inc.Shelton, CT USARapid Screening ofAdulteration inPomegranate Juice withApple Juice Using DSA/TOF with MinimalSample PreparationDownload Entire Application Note
  12. 12. Download Entire Application NoteTABLEOFCONTENTSIntroductionScreening methods for drugs of abusecurrently require long chromatographicmethods and sample preparation orimmunoassay techniques (EMIT) withconfirmation by GC/MS or LC/MS/MS.These methods can be time-consumingand laborious. The majority of urinescreening methods cover only a limitednumber of metabolites, since referencestandards are poorly available, making it difficult to keep up with the changing illicitdrug scene. Due to the variety of the illicit and abused drugs available, it is importantto monitor the entire spectral range, which is easily performed using a time-of-flight-mass spectrometer (TOF MS). The ability to analyze samples rapidly is desirable, asdrug seizures and patient screening may result in thousands of samples. A methodwas developed using the AxION®2 TOF MS integrated with the AxION Direct SampleAnalysis™(DSA™) system (Figure 1) for screening various classes of street seized, illicitdesigner drugs, drugs of abuse and abused human growth hormones in solid, liquidsas well as metabolites in urine of possible illicit drug offenders.This method enables fast screening and confirmation withminimal or no sample preparation using the AxION DSAsystem. We present a real life case study for the analysis of369 unknown drugs from seized pills, vials, powders andurine samples (Figure 2). The study shows the suitability ofMass Spectrometrya p p l i c a t i o n n o t eAuthorsSean Daugherty, Hayley CrowePerkinElmer, Inc.Seer Green, Beaconsfield,HP9 2FX United KingdomAutomated DirectSample Analysis(DSA/ToF) for theRapid Screening andConfirmation of IllicitStreet DrugsFigure 1: AxIoN DSA System
  13. 13. Download Application BriefTABLEOFCONTENTSFor a complete listing of our global offices, visit ©2012, PerkinElmer, Inc. All rights reserved. PerkinElmer®is a registered trademark of PerkinElmer, Inc. All other trademarks are the property of their respective owners.010563_01PerkinElmer, Inc.940 Winter StreetWaltham, MA 02451 USAP: (800) 762-4000 or(+1) 203-925-4602www.perkinelmer.comTOF MSDIrECt SAMPlE AnAlySISResults in secondsNo sample preparationNon destructiveForensics: Ethyl Centralite• DSA/TOF analysis on fabric identified gunshot residue by confirmation of ethyl centralite with accurate mass• 2% Dichloromethylene in methanol was infused at 10 µL/min and DSA/TOF was run in positive mode• The analysis was performed in 15 seconds with no sample preparation and external calibration• Residue analysis on fabric is important for forensic analysis of crime scenes. Modern gun powders use nitrocellulose and nitroglyercin as basic ingredients.
  14. 14. TABLEOFCONTENTSDownload Entire Application NoteIntroductionTime of flight (TOF) mass spectrometryprovides exact mass information andhigh sensitivity over a wide mass rangeenabling identification of unknowncompounds such as impurities. Using theexact mass capabilities and proprietaryTrapPulse™technology of the PerkinElmerAxION®2 TOF MS, we are able todescribe a workflow that allows us tofind impurities and identify them incommon over the counter drugs. Traditionalscanning instruments, such as quadrupolemass spectrometers, suffer a large loss in sensitivity when scanning over a widemass range. This loss in sensitivity does not occur with the AxION 2 TOF massspectrometer due to its fast sampling rates which enables us to detect impuritiesthat would otherwise be missed. The innovative TrapPulse mode of the AxION 2TOF MS further enhances its sensitivity, in this instance 8X, by collecting densepackets of ions before pulsing them into the flight tube. This allows us to easilydetect low level unknowns that may not be found in traditional TOF designs.In addition to the sensitivity over a wide dynamic range, the AxION 2 TOF MSprovides accurate mass enabled by real time lock mass, accurate isotope mea-surement, and mass resolution, all of which increases confidence for fast andaccurate identification of impurities. The enhanced mass accuracy and the abilityto determine precise isotope ratios provided by the AxION 2 TOF MS significantlyLiquid Chromatography/Mass Spectrometrya p p l i c a t i o n n o t eAuthorSharanya ReddyPerkinElmer, Inc.Shelton, CT USAIdentification ofImpurities UsingAccurate Mass,Sensitivity and WideDynamic Range of theAxION 2 TOF MS
  15. 15. TABLEOFCONTENTSIntroductionLactose is a very important pharmaceutical excipientused in tablet and inhalation products. It is prone toforming amorphous regions on processing however, andit can be problematical to characterize amorphic materialin a sample. Differential Mechanical Analysis (DMA)with material pocket is a method which can be usedto accurately determine very low levels of amorphouscontent in lactose (Royall 2005, Mahlin 2009), due to thehigh sensitivity of DMA to glass transitions. The materialpocket facilitates the analysis of lactose in the powderform, resulting in a very powerful tool for the analysis ofmixtures of crystalline and amorphous lactose.DMA works by applying an oscillating force to the material and the resultant displacement ofthe sample is measured. From this, the stiffness can be determined and the modulus and tan δcan be calculated. The modulus is a highly useful measure of the materials properties. Whenan oscillating stress is applied to a material in the DMA, the material becomes deformed, orstrained. The amplitude of the deformation is measured, and the ratio of the applied stress andthe resultant strain is termed the modulus. When a material goes through a transition such asa melt or recrystallization, that involves a dramatic change in the materials stiffness, a step-change will be observed in the modulus value. This indicates that the material has become stiffer(recrystallization) or less stiff (melting), and is a useful indicator of the materials structure duringheating. In a viscoelastic material, there will be two components to the modulus, one in phasewith the applied stress (the storage modulus), and one out of phase (the loss modulus). The ratioof the in phase and out of phase components of the modulus describes the damping propertiesof the material, and is termed tan δ. If tan δ is plotted against temperature a glass transition willnormally be observed as a peak since the material will absorb energy as it passes through theglass transition.The Application ofMesh Material Pocketsin DMA Analysis ofAmorphous andCrystalline LactosePowdersDynamic Mechanical Analysisa p p l i c a t i o n n o t eAuthorsFrederick J. WarrenRosa PandolfoGary P. MartinPaul G. RoyallKing’s CollegeLondon, U.K.Kevin P. MenardRobert PackerPerkinElmer, Inc.Shelton, CT USADownload Entire Application Note
  16. 16. TABLEOFCONTENTSPerkinElmer, Inc.940 Winter StreetWaltham, MA 02451 USAP: (800) 762-4000 or(+1) 203-925-4602www.perkinelmer.comFor a complete listing of our global offices, visit ©2013, PerkinElmer, Inc.All rights reserved. PerkinElmer® is a registered trademark of PerkinElmer, Inc.All other trademarks are the property of their respective owners.011164_01USEFUL LINKSView previous issues of our Spotlight on Applications e-Zine• Volumes 1-14• Food Beverage Special Edition• Environmental Special EditionAccess our application archivesBy Industry:• Consumer Products• Energy• Environmental• Food, Beverage Nutraceuticals• Forensics• Lubricants• Pharmaceutical Development Manufacturing• Polymers/Plastics• Semiconductor ElectronicsBy 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• Thermal Analysis• UV/Vis UV/Vis/NIRIntroducing AxION® iQT™GC/MS/MS, revolutionarytechnology that combinestriple quad and Q-TOFcapabilitiesinoneinstrument!Meet the NewTitan MPS™ MicrowaveSample Preparation System