Method development and validation for determination of pharmaceuticals and personal care products in river water and sewage
Pharmaceuticals and Personal Care Products (PPCPs) are classified as the new emerging class of pollutants by the United States Environmental Protection Agency (U.S. EPA) recently. Its ubiquitous nature coupled with its high persistency in the environment is alarming. Moreover, some PPCPs are...
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| Format: | Thesis |
| Language: | English |
| Published: |
2012
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| Subjects: | |
| Online Access: | http://psasir.upm.edu.my/id/eprint/67597/1/FPAS%202013%2016%20IR.pdf |
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| Summary: | Pharmaceuticals and Personal Care Products (PPCPs) are classified as the
new emerging class of pollutants by the United States Environmental
Protection Agency (U.S. EPA) recently. Its ubiquitous nature coupled with its
high persistency in the environment is alarming. Moreover, some PPCPs are
endocrine disrupting compounds responsible for feminization of male fishes
via production of viltellogenin. Occurrences of antibiotics in the environment
induce high bacterial resistance. PPCPs were widely manufactured and
administered in Malaysia but little or no quantification was carried out. Lack
of data could be attributed to the absence of a recognized, comprehensive
and conclusive method for PPCPs analysis. As such, this method aims to
provide a robust and sensitive method for identification and quantification of PPCPs in river water, Sewage Treatment Plant (STPs) influent, intermittent
and effluent. This method is specially formulated for simultaneous extraction,
detection and quantification of multi-classes PPCPs in a 25 minutes run-time.
This is a pioneering method for quantification of acetaminophen,
sulfamethoxazole, diclofenac, atenolol, metoprolol, DEET and oxybenzone in
Atmospheric Pressure Chemical Ionisation (APCI) mode. Method had been
validated for high repeatability and reproducibility; Relative Standard
Deviations (RSD) for both was less than 10%. Quantification of PPCPs is
often a trace analysis; thus, a good sensitivity is needed. As such, Instrument
Quantification Limits (IQLs) for PPCPs were in the range of 0.05-1.0 μg/L;
meanwhile, Method Quantification Limits (MQLs) for ultrapure water were
within 0.3-15 ng/L. In addition, Solid Phase Extraction (SPE) recoveries were
above 75% for most PPCPS demonstrating good accuracy. Lower matrix
suppression in APCI mode had enabled quantifying PPCPs in complex
matrices producing lower baseline chromatograms and sharper peaks
resolutions. Subsequently, the method was applied to investigate
environmental occurrences of PPCPs. Twelve out of eighteen PPCPs were
detected in river water samples. Five PPCPs were quantified above 1000
ng/L; they were caffeine, estradiol, estriol, estrone and naproxen. On the
other hand, three sewage treatment plant (STPs) with different operational
mechanisms were sampled. Natural hormones (estradiol, estriol, estrone and
progesterone) and personal care products (caffeine, DEET and oxybenzone)
constituted majority of influents. Highest detected in influent was caffeine
whose mean concentration was 14858.4 ng/L. Thirteen PPCPs were
detected in all STP effluents. Highest concentration in effluent was estriol whose mean concentration was 2160.6 ng/L. In a nutshell, PPCPs were not
efficiently removed by Malaysian STPs. Thereafter, Environmental Risk
Assessments (ERA) was used to evaluate possible aquatic toxicities in
Langat River. High risks of acute toxicities were found for naproxen and
sulfamethoxazole. Several PPCPs exhibited high chronic toxicities namely
diclofenac, estradiol, ethynylestradiol, estriol, estrone, and sulfamethoxazole.
Naproxen exhibited medium risk. Metoprolol and DEET exhibited low chronic
risk. Immediate reduction measures were demanded for four steroid
hormones; they were estradiol, estriol, estrone and ethynylestradiol. |
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