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  • A poly(alkyl methacrylate-divinylbenzene-vinylbenzyl trimethylammonium chloride) monolithic column for solid-phase microextraction.

A poly(alkyl methacrylate-divinylbenzene-vinylbenzyl trimethylammonium chloride) monolithic column for solid-phase microextraction.

Journal of chromatography. A (2015-04-15)
Wan-Ling Liu, Stephen Lirio, Yicong Yang, Lin-Tai Wu, Shu-Ying Hsiao, Hsi-Ya Huang
ABSTRACT

In this study, an organic polymer monolithic columns, which were prepared via in situ polymerization of alkyl methacrylate-ester (AMA), divinylbenzene (DVB) and vinylbenzyl trimethylammonium chloride (VBTA, charged monomer), were developed as adsorbent for solid-phase microextraction (SPME). Different parameters affecting the extraction efficiency for nine (9) non-steroidal anti-inflammatory drugs (NSAIDs) such as the ratio of the stearyl methacrylate (SMA) to DVB monomer, column length, sample pH, extraction flow rate and desorption solvent were investigated to obtain the optimal SPME condition. Also, the permeability for each poly(AMA-DVB-VBTA) monolithic column was investigated by adding porogenic solvent (poly(ethylene glycol), PEG). Using the optimized condition, a series of AMA-based poly(AMA-DVB-VBTA) monolith columns were developed to determine the effect the extraction efficiency of NSAIDs by varying the alkyl chain length of the methacrylate ester (methyl-, butyl-, octyl-, or lauryl-methacrylate; (MMA, BMA, OMA, LMA)). Results showed that decreasing the AMA chain length increases the extraction efficiency of some NSAIDs (i.e. sulindac (sul), naproxen (nap), ketoprofen (ket) and indomethacin (idm)). Among the poly(AMA-DVB-VBTA) monolithic columns, poly(BMA-DVB-VBTA) showed a highly repeatable extraction efficiency for NSAIDs with recoveries ranging from 85.0 to 100.2% with relative standard deviation (RSD) less than 6.8% (n=3). The poly(BMA-DVB-VBTA) can also be reused for at least 50 times without any significant effect in extraction efficiency for NSAIDs. Finally, using the established conditions, the poly(BMA-DVB-VBTA) was used to extract trace-level NSAIDs (100μgL(-1)) in river water with good recoveries ranging from 75.8 to 90.8% (RSD<14.9%).

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME Portable Field Sampler, coating CAR/PDMS
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with manual holder, needle size 23 ga
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 23 ga
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME Portable Field Sampler, coating PDMS
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 24 ga
Supelco
SPME Sampling Stand, for use with 4 mL vials
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 7 μm(PDMS, needle size 24 ga, for use with autosampler
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with manual holder, needle size 24 ga
Supelco
SPME fiber assembly polyacrylate (PA), df 85 μm(PA, for use with autosampler, needle size 24 ga
Supelco
SPME Portable Field Sampler, coating PDMS/DVB
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 30 μm(PDMS, needle size 24 ga, for use with manual holder
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 100 μm(PDMS, for use with autosampler, needle size 23 ga
Supelco
SPME Sampling Stand, for use with 15 mL vials
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), df 30 μm(PDMS, needle size 24 ga, for use with autosampler
Sigma-Aldrich
1-Methyl-2-pyrrolidinone, anhydrous, 99.5%
Sigma-Aldrich
Indomethacin, 98.5-100.5% (in accordance with EP)
Sigma-Aldrich
Sulindac, ≥98.0%
Sigma-Aldrich
Diclofenac sodium salt
Sigma-Aldrich
Indomethacin, meets USP testing specifications
Supelco
SPME fiber assembly Polydimethylsiloxane (PDMS), metal alloy fiber, df 100 μm(PDMS, needle size 23 ga, for use with autosampler
Supelco
SPME-OC Fiber Assembly, Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 75 μm(Coating thickness includes 65 μm coating + 10 μm OC (overcoating), needle size 23 ga, pkg of 3 ea, fiber L 1 cm
Sigma-Aldrich
Ketoprofen, meets USP testing specifications
Supelco
SPME fiber assortment kit 5, needle size 23 ga, for use with autosampler
Sigma-Aldrich
Ibuprofen, ≥98% (GC)
Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, ≥97%
Sigma-Aldrich
Ketoprofen, ≥98% (TLC)
Sigma-Aldrich
Flurbiprofen, cyclooxygenase inhibitor