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Pharmaceuticals and Personal Care Products Analysis in Bottled, Tap and Surface Water Using Two-dimensional Liquid Chromatography Mass Spectrometry (2D LC/MS/MS)
Oral Presentation
Prepared by C. Mallet
Waters Corporation, 34 Maple St, Milford, MA, 01757, United States
Contact Information: claude_mallet@waters.com; 508-482-3045
ABSTRACT
Since 2000, there has been increasing concern regarding the presence of pharmaceuticals and personal care products (PPCP’s) in water bodies throughout the world. The effects of these emerging contaminants on human health or their potential impact on the environment are not yet fully understood. The main analytical challenge for the analysis of PPCP’s is linked to their wide chemical diversity, encompassing many classes and structures. In addition, the complexity of the water samples requiring analysis can be very diverse. It is therefore critical to ensure a robust, reproducible multi-residue LC-MS/MS protocol is employed.
Extraction protocols used in conjunction with single dimension chromatography platforms (LC/MS/MS) are optimized to reach LOQ’s at trace levels (sub ppb), which often times are below detection capabilities of currently available detectors (optical or destructive). Therefore, a sample enrichment step is usually included in the extraction protocol to reach acceptable quantification limits. However, it typically comes at a price with hour long extraction processes, large sample quantities, and resources.
Multi-dimension chromatography offers a wide range of options; one in particular is the large volume injection capability for aqueous and organic extracts. This configuration brings drastic time reduction during sample preparation. The traditional hours-long macro-extraction method is reduced to micro-extraction scale. In this application, a 20 PPCP’s mix was extracted from a 20 mL sample volume (bottled, tap and surface) with a total extraction time of 15 minutes. The final eluate (1 mL MeOH) was directly transferred into a 2 mL vial, thus eliminating the evaporation and reconstitution step.
This micro extraction protocol gave excellent performance, with a 1 ppt detection limit (LOD) and good linearity (0.995 R2 with 1-100 ppt calibration curve). The majority of PPCPs gave recovery values for bottled, tap and surface water sample in the 90% to 108% range.
Oral Presentation
Prepared by C. Mallet
Waters Corporation, 34 Maple St, Milford, MA, 01757, United States
Contact Information: claude_mallet@waters.com; 508-482-3045
ABSTRACT
Since 2000, there has been increasing concern regarding the presence of pharmaceuticals and personal care products (PPCP’s) in water bodies throughout the world. The effects of these emerging contaminants on human health or their potential impact on the environment are not yet fully understood. The main analytical challenge for the analysis of PPCP’s is linked to their wide chemical diversity, encompassing many classes and structures. In addition, the complexity of the water samples requiring analysis can be very diverse. It is therefore critical to ensure a robust, reproducible multi-residue LC-MS/MS protocol is employed.
Extraction protocols used in conjunction with single dimension chromatography platforms (LC/MS/MS) are optimized to reach LOQ’s at trace levels (sub ppb), which often times are below detection capabilities of currently available detectors (optical or destructive). Therefore, a sample enrichment step is usually included in the extraction protocol to reach acceptable quantification limits. However, it typically comes at a price with hour long extraction processes, large sample quantities, and resources.
Multi-dimension chromatography offers a wide range of options; one in particular is the large volume injection capability for aqueous and organic extracts. This configuration brings drastic time reduction during sample preparation. The traditional hours-long macro-extraction method is reduced to micro-extraction scale. In this application, a 20 PPCP’s mix was extracted from a 20 mL sample volume (bottled, tap and surface) with a total extraction time of 15 minutes. The final eluate (1 mL MeOH) was directly transferred into a 2 mL vial, thus eliminating the evaporation and reconstitution step.
This micro extraction protocol gave excellent performance, with a 1 ppt detection limit (LOD) and good linearity (0.995 R2 with 1-100 ppt calibration curve). The majority of PPCPs gave recovery values for bottled, tap and surface water sample in the 90% to 108% range.