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Analysis of trace-level nitrated polycyclic aromatic hydrocarbons in water samples by solid-phase microextraction with gas chromatography and mass spectrometry.

Journal of separation science (2018-04-03)
Jijie Kong, Mengshu Han, Ying Liu, Huan He, Zhanqi Gao, Qiming Xian, Shaogui Yang, Cheng Sun, Shiyin Li, Limin Zhang
ABSTRACT

A solid-phase microextraction coupled with gas chromatography and mass spectrometry method has been developed for the determination of ten nitrated polycyclic aromatic hydrocarbons in water samples. Five different kinds of commerical fibers were used to compare the extraction efficiency, including 65 μm polydimethylsiloxane/divinylbenzene, 100 μm polydimethylsiloxane, 30 μm polydimethylsiloxane, 7 μm polydimethylsiloxane, and 85 μm polyacrylate fibers. Five factors were also selected to optimize conditions, including extraction temperature, time, stirring speed, salt concentration, and headspace volume. Taguchi design was applied to design the experiments and obtain the best parameters. The results show that 65 μm polydimethylsiloxane/divinylbenzene fiber directly immersed into aqueous solution for 35 min at 55°C with a constant stirring rate of 1150 rpm were the optimal conditions. Under these conditions, the limits of quantification were 0.007-0.063 μg/L, and the relative standard deviation based on six replicates ranged from 2.8 to 9.5%. The spiked recoveries ranged from 69.1 to 110.1%. Intra- and inter day relative standard deviations at three concentration levels were less than 12%, and the recoveries were 66.4-111.5%. The proposed method is reliable for analyzing nitrated polycyclic aromatic hydrocarbons in different water samples.

MATERIALS
Product Number
Brand
Product Description

Supelco
SPME fiber assortment kit 5, needle size 23 ga, for use with autosampler
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SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), for use with autosampler
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SPME fiber assembly, Carbowax-Polyethylene Glycol (PEG) Coating, needle size 23 ga, df 60 μm (PEG), metal alloy fiber, for use with manual holder
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SPME StableFlex fiber assortment kit, for use with autosampler, needle size 24 ga
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SPME fiber assortment kit 2, for use with manual holder, needle size 24 ga
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SPME fiber assortment kit 4, for use with autosampler, needle size 23 ga
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SPME fiber assortment kit 2, for use with autosampler, needle size 23 ga
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 23 ga, PDMS/DVB StableFlex, for use with autosampler
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SPME StableFlex fiber assortment kit, needle size 23 ga, for use with autosampler
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SPME fiber assortment kit 1, for use with autosampler, needle size 23 ga
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with autosampler
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, StableFlex, for use with manual holder
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), fused silica fiber, df 65 μm (PDMS/DVB), for use with manual holder, needle size 23 ga
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SPME StableFlex fiber assortment kit, for use with manual holder
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), needle size 24 ga, for use with autosampler
Supelco
SPME fiber assortment kit 1, for use with manual holder, needle size 24 ga
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SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga, metal alloy fiber
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SPME fiber assortment kit 4, for use with manual holder, size 24 ga
Supelco
SPME fiber assortment kit 1, for use with autosampler, needle size 24 ga
Supelco
SPME Fiber Assembly Polydimethylsiloxane/Divinylbenzene (PDMS/DVB), df 65 μm (PDMS/DVB), for use with autosampler, needle size 23 ga
Supelco
SPME fiber assortment kit 4, for use with autosampler, size 24 ga
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SPME fiber assortment kit 2, for use with autosampler, size 24 ga
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IonSense® PDMS/DVB SPE-it Tips, pkg of 96 ea
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SPME LC Tips, C18, tray of 96 ea
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IonSense® C18 SPE-it Tips, pkg of 96 ea
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SPME LC Tips, PDMS/DVB, pkg of 96 ea
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SPME fiber assembly Polydimethylsiloxane (PDMS), metal alloy fiber, df 100 μm (PDMS), needle size 23 ga, for use with autosampler
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SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with autosampler
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SPME fiber assembly Divinylbenzene/Carboxen/Polydimethylsiloxane (DVB/CAR/PDMS), needle size 23 ga, StableFlex, for use with manual holder or autosampler, fiber L 2 cm