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Pharma Notes

Pharma Notes

Online SPE HPLC/MS/MS has also been used to analyze a variety of trace organics in water. These include herbicides, pesticides, pharmaceuticals, estrogens, and glyphosate in potable water. Sarah Gledhill of SouthEast Water (UK) reports on a validated online SPE LC/MS/MS method for detection of 17 chlorinated phenoxy acid herbicides and pentachlorophenol (PCP) in surface and treated water, using only 1.5 mL of sample.9

This method delivers <10 ng/L (ppt) limits of detection (LODs), as well as recoveries >95 per cent for most of the compounds. In addition to a reduction in sample volume, this method provides faster results at lower cost. The solid phase extraction cartridges are reusable, and less solvent is used for extraction of the sample. Finally, the results are more reproducible than their older method based on manual SPE, because the system is fully automated and less prone to operator error. This method meets the performance requirements set by the UK Drinking Water Inspectorate for standard deviation, bias, recovery, and total error and is accredited by the United Kingdom Accreditation Service (UKAS).

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Q-TOF Accurate Mass analysis enables highly sensitive and untargeted screening of pharmaceuticals in water

Mike Thurman and Imma Ferrer at the University of Colorado demonstrated that a quadrupole time-offl ight mass spectrometer (Q-TOF MS) can provide high confi dence identifi cation and quantitation of pharmaceuticals, enabling an untargeted LC/ MS screening method that has been used to characterize more than 100 pharmaceuticals and their metabolites in water sources at concentrations as low as parts per trillion10 (Table 2). Sophisticated software tools for molecular feature extraction, formula generation, molecular structure correlation, and accurate mass database matching are key to the success of the method. This approach is particularly useful for separating and identifying isobaric and isomeric compounds that can be diffi cult to analyze using other methods.

Mobile analysis can be used effectively to rapidly assess drinking water quality

Circumstances can often dictate the need for onsite analysis to immediately confi rm the safety of surface and drinking water. Such a need arose after a recent earthquake in China. Agilent Technologies was requested to provide onsite water quality monitoring, as rapid and reliable lab-quality results in the fi eld were necessary in order to make decisions to avoid a national emergency from contaminated drinking water.

The Agilent 5975T LTM GC/MSD, a mobile combination gas chromatograph/mass selective detector (GC/ MSD) confi gured with a purge and trap concentrator and low thermal mass technology, was used as a testing station in this crisis.11 Although portable, it provided the accuracy and sensitivity required to assure compliance with regulatory standards for drinking water safety (Figure 2).

A method was developed on this portable system to rapidly analyze for 22 trace volatile organic pollutants that are regulated in drinking water. While routine cycle time was reduced to fi ve to 10 minutes, compared to more than 30 minutes with traditional laboratory methods, the minimum detection limits varied between 0.090.14 μg/l (ppb) for all 22 compounds These levels are below the acceptable detection limits for these compounds in drinking water in China. This method provides results with high sensitivity, accuracy, sensitivity, and reproducibility similar to results that can be obtained in a stationary lab, providing the versatility for analyses in remote disaster locations.

Conclusion

Modern society generates a plethora of waste products containing a wide range of organic chemicals that are clearly making their way into surface and drinking water. These compounds are often present in trace amounts, even parts per trillion, and their impact on the environment and human health are unknown.

Regulatory agencies worldwide are making efforts to characterize the nature and concentrations of these compounds so that their threat to the environment and human health can be accurately assessed. These efforts require new technologies and methods to assure success in a meaningful timeframe. Recent advances in automated online sample enrichment, more sensitive and faster scanning mass spectrometers, Q-TOF and accurate mass software tools, and mobile analysis systems are helping to meet this challenge. Together they can reduce the time and sample volume needed to assess water sources, while providing accurate and reproducible detection of >200 trace organic contaminants simultaneously, at parts per trillion (ng/L) concentrations.

References

1. Anumol T., Merel S., Clarke B. O.,

Snyder S. A. Ultra high performance liquid chromatography tandem mass spectrometry for rapid analysis of trace organic contaminants in water. Chem

Cent J. Jun 18;7(1):104 (2013). 2. Kidd K. A., Blanchfi eld P. J., Mills

K. H., Palace V. P., Evans R. E.,

Lazorchak J. M., Flick R. W. Collapse of a fi sh population after exposure to a synthetic estrogen.

Proc Natl Acad Sci U S A. 104, 8897-8901 (2007). 3. Drugs in the drinking water, an

Associated Press Investigation: http://hosted.ap.org/specials/interactives/pharmawater_site/. 4. Arvai A., Flecka G., Jasim, S.

Melcer H., Laitta M. T. Protecting our great lakes: assessing the effectiveness of wastewater treatments for the removal of chemicals of emerging concern.

Water Qual Res J Can In Press, doi:10.216/wgrjc 2013.104. 5. Blair B. D., Crago J. P., Hedman

C. J., Klaper R. D., Pharmaceuticals and personal care products found in the Great Lakes above concentrations of environmental concern. Chemosphere 93, 2116-2123 (2013). 6. Unregulated Contaminant Monitoring Rule 3 (UCMR3),http:// water.epa.gov/lawsregs/relesreg/ sdwa/ucmr/ucmr3/index.cfm 7. Pollutants in Urban Waste Water and Sewage Sludge, http://ec.europa.eu/environment/ waste/sludge/pdf/sludge_pollutants_xsum.pdf 8. Anumol T., Snyder S., Mohsin S.

B. Sensitive LC/MS Quantitation of Trace Organic Contaminants in Water with Online SPE Enrichment. Agilent Technologies

Application Note 5991-1849EN (2013). 9. Gledhill, S. High Sensitivity Detection of Pesticides in Water

Using Online SPE Enrichment.

feature

Agilent Technologies Application

Note 5991-0871EN (2012). 10. Ferrer I., Thurman E. M. High

Resolution Mass Spectrometry (LC/Q-TOF/MS) for the Detection of Pharmaceuticals in Water.

Agilent Technologies Application

Note 5991-3261 (2013). 11. Cooperation with the China

Academy of Urban Planning and

Design for Field VOC Measurement of Drinking Water Sources with the Agilent 5875T LTM GC/

MSD. Agilent Technologies Application Note 5991-3140EN (2013).

Mr. Weitzel is the Agilent Global Environmental Market Development Manager. Before being employed by Agilent, Joe had been employed as a municipal water utility chemist and the lab manager for an environmental contract testing laboratory. Joe has been with Agilent since 1984 in various sales and marketing positions.

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new Products

Pumps

RC_lab_new:Layout 1 12/19/2012 10:01 AM Page 1

The new Masterflex® L/S® Compact Pumps with Miniflex™ Pump Head from Cole-Parmer is a complete system which includes a pump head and drive. Created for transferring, sampling or filling applications in laboratories and research settings, the new peristaltic pump system delivers repeatable low flow rates with flow ranges of 1.8 to 220 mL/min (depending on the model and tubing size selected). It operates with continuous tubing, eliminating leakage and the need for fittings or connections, thus providing a cleaner fluid path. Users can select from several formulations of tubing. Automatic tubing retention makes the tube loading quick and painless—it takes less than 15 seconds. The stackable Masterflex pump operates with single-turn speed control for forward or reversible pumping and maintains speed setting when the pump is turned off. Select from single-channel and dual-channel models.

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Workstation

Hamilton Robotics launches the Decapping Microlab® STAR workstation, a fully automated tube tracking, decapping and recapping workstation. It includes eight decapping modules for safe and secure sample preparation. By incorporating lab automation, researchers can speed up time to results and spend more time analyzing data instead of managing and monitoring complex workflows. In addition to decapping and recapping, the STAR Workstation transports

tubes, mixes liquids in tubes, pipettes and tracks samples. Although timing depends on pipetting volumes, the entire process of tube and cap handling can be accomplished within a few minutes. Up to two Decapping Modules can be placed on a STAR deck and are served by four twister channels on a slim arm, with up to eight 1 mL or four 5 mL channels on an additional slim arm. The decapping modules are completely controlled and monitored through VENUS software so that all steps can be tracked and handled automatically, thus increasing process reliability. The system can accommodate tubes with a diameter of 15 to 38 mm, with caps up to six mm larger in diameter than the tube, to ensure robust and versatile handling. Web: www.hamiltonrobotics.com

Molecular Arrays

Oxford Gene Technology (OGT) has expanded its range of research-validated CytoSure Molecular Arrays to investigate DNA copy number variation (CNV) underlying a variety of genetic disorders. Designed and optimised in collaboration with experts at Emory Genetics Laboratory (Atlanta, GA), the arrays are the ideal complement to DNA sequencing, providing a particularly powerful tool for investigating the variety of aberrations underlying genetic disorders. The expanded CytoSure Molecular Array portfolio now enables detection of CNV in genes associated with over 20 genetic disorders, including cardiovascular, inherited eye, intellectual disability and neuromuscular disorders, as well as a range of inherited cancers. In addition, genes covering each disorder can be combined to create bespoke custom arrays, or further customised by the addition of novel content to suit each individual research project. For the easy extraction of results from aCGH data, all CytoSure Molecular Arrays are supplied with OGT’s CytoSure Interpret Software. Web: www.ogt.com

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