A Highly Sensitive MRM-Based Method for Detection and Quantitation of Seven Pharmaceuticals and Personal Care Products (PPCPs) in Surface Water

Significance of the Topic

The presence of pharmaceuticals and personal care product residues in surface water is an emerging environmental and public health issue. These compounds persist through conventional wastewater treatment and may act as endocrine disruptors at trace concentrations, prompting the need for sensitive monitoring methods.

Objectives and Study Overview

This work describes the development of a direct analysis method using a triple quadrupole LC MS MS system to detect and quantify seven priority PPCPs at low parts per trillion levels in treated and reservoir water without pre concentration or enrichment steps.

Methodology and Instrumentation

A Shimadzu LCMS 8060 triple quadrupole coupled to a Nexera UHPLC was employed. Separation used a pentafluorophenyl column with a water acetonitrile gradient containing 0.1 percent formic acid at a flow rate of 0.3 milliliter per minute and column temperature of forty degrees Celsius. An injection volume of ten microliters was applied. Electrospray ionization in both positive and negative modes was used. Key source parameters included an interface temperature of three hundred degrees, desolvation line temperature of two hundred fifty degrees, heat block at four hundred degrees, nebulizing gas at three liters per minute and drying gas at five liters per minute.

Sample preparation consisted of serial dilutions of stock solutions in Milli Q water for calibration. Treated wastewater effluent and reservoir water samples were analyzed directly by injection without further cleanup.

Results and Discussion

MRM transitions were optimized with two transitions per compound for quantitation and confirmation. Linear calibration ranges spanned from one to one thousand nanograms per liter, achieving correlation coefficients above 0.99 for most analytes. Limits of detection ranged from one nanogram per liter for gemfibrozil up to thirteen and a half nanograms per liter for ketoprofen. Repeatability at concentrations near the quantitation limits showed relative standard deviations below eight percent. Analysis of real water samples detected triclosan at about ten point nine nanograms per liter in both treated and reservoir water. A minor signal for gemfibrozil at around point five nanograms per liter was observed below the method detection limit. Spiked samples confirmed reliable detection and quantitation at low tens of nanograms per liter.

Benefits and Practical Applications

This direct MRM method offers rapid throughput and high sensitivity without time consuming sample concentration. It is suitable for routine monitoring of trace level PPCPs in environmental and drinking water quality control laboratories.

Future Trends and Opportunities

Advances may include coupling on line solid phase extraction for further sensitivity enhancement, expansion of target lists to cover emerging contaminants, integration with high resolution mass spectrometry for non target screening, and automation of data processing for high throughput environmental surveillance.

Conclusion

A robust LC MS MS method on a triple quadrupole instrument has been established, enabling direct quantitation of seven key PPCPs at low nanogram per liter levels in surface water samples without pre concentration. The approach demonstrates strong linearity precision and low detection limits, supporting environmental monitoring and regulatory compliance efforts.

Reference

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4. Pryor K Byrne J Lieberman R Gilles C LC MS MS Method for Evaluation of PPCPs in Environmental Water ASMS 2016 MP169 2016
5. Xing J Wu J Zhan Z Fully Automated Multiple Injection On line SPE LC MS MS Method for Analysis of Trace Level Drug Residues in Water ASMS 2012