One-Step Extraction and Concentration for Identifying Pharmaceuticals and Personal Care Products in Water, Biosolids and Solids

Introduction
Over the last decade the use of Pharmaceuticals and Personal Care Products (PPCPs) has doubled in the United States. As a result, PPCPs have entered the environment through both human activity and as by-products from manufacturing, agricultural activities, medical use and veterinarian facilities. PPCPs are usually introduced into the environment through the disposal of unused medications into sewer systems and trash. PPCPs tend to be water soluble and do not evaporate under normal temperatures, which is why they end up in soil and water. The full effects of PPCPs on the environment are not fully understood and there is concern about the potential threat they pose to the food chain. Because of the high solubility of most PPCPs, aquatic organisms are most vulner-able. The classes of pharmaceuticals found in these organisms have been linked to slow growth in frogs and the increased feminization of exposed fish. The scope of human exposure to PPCPs from the environment is complicated and increased monitoring is occurring to determine the effect on humans of long-term, low-level exposure to PPCPs.

Due to their persistent nature and toxicity, monitoring water sources for PPCPs is a growing priority for both government agencies and consumers. The following procedure outlines the fully automated, sample-to-vial extraction and concentration of water matrices for the detection of these compounds in one rapid and efficient process.

Instrumentation and Consumables
FMS, Inc. PowerPrepTM SPE system (Solid Phase Extraction)
FMS, Inc. PowerVapTM Concentrator
FMS, Direct-to-Vial concentrator tubes
1 gram Waters OasisTM HLB cartridge UPLC, LC/MS.

Procedure: Sample Prep Extraction and Concentration
PowerPrep SPE
1. Condition the cartridge with 10 mL of methanol
2. Condition the cartridge with 10 mL of water
3. Load the 1 liter water sample at 100 mL/min
4. Rinse the cartridge
5. Dry the cartridge with nitrogen and vacuum for 20 minutes
6. Elute the cartridge with 15 mL of methanol base fraction
7. Elute the cartridge with 15 mL of methanol 2% formic acid
8. The Fractions are directly eluted to the PowerVap Concentrator system

PowerVap Direct-to-Vial Concentration
Pre-heat temp: 40 °C.
Pre-heat time: 10 minutes
Heat in sensor mode: 50 °C
Nitrogen pressure: 15 PSI
Sensor 1 mL Direct to GC vial

Results

Table 1 shows the mean recoveries from the five extracts after analysis from several types of PPCPs in Water.

Conclusions
Analysis of the LC/MS data demonstrates excellent recoveries and reproducibility from a traditionally difficult sample matrix. Adding to the efficiency was the use of nitrogen and vacuum to dry the cartridge and a water free extract that enables a fast concentration step with no loss of analytes. The extract takes 45 minutes to concentrate using the PowerPrep™ SPE system compared to all other drying methods. View video here.

Using the automated, one-step SPE and Direct-to-Vial Concentration tubes from FMS, Inc. eliminates error-prone manual or semi-automated steps from the sample prep process. No sample transfer was necessary, which allowed the sample to be extracted and automatically sent to the PowerVap Concentrator where the final extract is concentrated directly to a vial for LC/MS analysis. This capability eliminated human error, saved time and increased efficiency while producing reproducible and consistent recoveries.

For more information on the SPE system