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A new analytical method to determine non-steroidal anti-inflammatory drugs in surface water using in situ derivatization combined with ultrasound-assisted emulsification microextraction followed by gas chromatography-mass spectrometry.

Talanta (2014-08-17)
Cheong Hoon Lee, Yujin Shin, Min Woo Nam, Kyung Min Jeong, Jeongmi Lee
ABSTRACT

Because of the high stability and potential toxic effects of non-steroidal anti-inflammatory drugs (NSAIDs), it is important to closely monitor their concentrations in the environment using a sensitive analytical method. In this study, a simple, rapid, efficient, and sensitive analytical method based on gas chromatography-mass spectrometry (GC-MS) was developed to determine the levels of seven common NSAIDs in various types of surface water. To simplify sample preparation, in situ derivatization using methyl chloroformate was combined with ultrasound-assisted emulsification microextraction. For selection and optimization of significant variables, experiments were statistically designed using Plackett-Burman design and central composite design. The resulting optimal conditions for derivatization and extraction were 100 μL of chloroform (extraction solvent), 10.0 mL of sample, and 240 μL of pyridine (catalyst as a base in derivatization). The optimized sample preparation coupled with optimized GC-MS analysis in selected ion monitoring mode provided good linearity from 0.010 to 5.0 ng mL(-1), and a limit of detection between 0.0050 and 0.010 ng mL(-1), good intra-day and inter-day precision (0.30-6.3% and 5.1-9.5%, respectively), and good accuracy (relative recovery; 91-117% at 0.20 ng mL(-1) and 77-105% at 2.5 ng mL(-1)). Compared with previously reported methods, the current method requires a small volume of sample and simple sample preparation steps for sensitive determination of NSAID levels using a conventional GC-MS system. The method was successfully applied to determine the levels of seven common NSAIDs in various types of surface water.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Toluene, anhydrous, 99.8%
Sigma-Aldrich
Pyridine, anhydrous, 99.8%
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Ethyl acetate, anhydrous, 99.8%
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Chloroform, contains 100-200 ppm amylenes as stabilizer, ≥99.5%
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Diethyl ether, contains 1 ppm BHT as inhibitor, anhydrous, ≥99.7%
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Ethyl acetate, ACS reagent, ≥99.5%
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Chloroform, anhydrous, ≥99%, contains 0.5-1.0% ethanol as stabilizer
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Ethyl acetate, suitable for HPLC, ≥99.7%
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Cyclohexane, anhydrous, 99.5%
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Diethyl ether, suitable for HPLC, ≥99.9%, inhibitor-free
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Diethyl ether, contains BHT as inhibitor, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
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Toluene, ACS reagent, ≥99.5%
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Diethyl ether, anhydrous, ACS reagent, ≥99.0%, contains BHT as inhibitor
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Ethyl acetate, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.5% (GC)
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Pyridine, ACS reagent, ≥99.0%
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Chloroform, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%, contains amylenes as stabilizer
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