LC–MS-MS Measurement of EPA Method 1694 Pharmaceuticals and Personal Care Products in Water

June 1, 2015
Shimadzu Scientific Instruments, Jeremy Post

The Application Notebook

Issue 0

This method increases sensitivity and reduces data acquisition time for a subset of pharmaceuticals and personal care products from the original EPA Method 1694 specifications.

This method increases sensitivity and reduces data acquisition time for a subset of pharmaceuticals and personal care products from the original EPA Method 1694 specifications.

Both pharmaceuticals and personal care products have increasingly passed into our nation's waters since their first use. Though present in low concentrations, some of the thousands of these chemical species are suspected of impacting both plant and animal health. To effectively study the impacts of these chemicals on the environment, a sensitive and selective analytical method utilizing a LCMS-8050 UHPLC-triple quadrupole mass spectrometer demonstrated here can monitor these species at low levels. In addition to improved sensitivity, the ultrafast instrument operating speed utilizes methods that are 7–8 times shorter than those in the original work.

Experimental Conditions

Method 1694 measures analytes from many disparate compound classes and therefore subdivides each sample into groups utilizing four unique extractions. This work demonstrates analytes from groups 1 (acidic extraction, positive polarity) and 3 (acidic extraction, negative polarity). The mobile phases best suited for their measurement differ, requiring two methods. An Eclipse Plus C18 1.8µ 2.1 × 150 mm column was used in both methods, flowing at 0.3 mL/min, 40 °C. Source temperatures including a heated ESI probe, heat block, and desolvation line along with heating, nebulizer, and drying gas flows and interface voltages were optimized. The autosampler tray was kept at 4 °C.

Results

Using mobile phases dedicated to both low and high pH in two methods improved the sensitivity for each analyte significantly (data not shown). Table I provides a comparison of method parameters and minimum levels of quantitation (ML) (1) together with the range of concentrations included in the calibration curve for each analyte with its coefficient of determination.

Conclusions

Utilizing Method 1694 as a foundation, pharmaceuticals and personal care products can be sensitively quantitated on the Shimadzu LCMS-8050

Reference

(1) http://water.epa.gov/scitech/methods/cwa/bioindicators/upload/2008_01_03_methods_method_1694.pdf

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