Application of Octadecyl Ionic Liquid Hybrid Solid-phase Microextraction Monolithic Column in the Detection of Polycyclic Aromatic Hydrocarbons in Coffee†

doi:10.7503/cjcu20170068

Abstract

Abstract:

Ionic liquid of 1-octadecyl-3-(γ-triethoxysiliconpropyl)imidazole bromide(C₁₈IL) was synthesized and then used as a functional monomer to produce the in-tube solid microextraction monolithic column(C₁₈IL in-tube SPME) via sol-gel reaction. After that, five polycyclic aromatic hydrocarbons(PAHs), naphthalene, fluorine, phenanthrene, fluoranthene and pyrene, were employed as probe analytes to evaluate the preparation method of the column and optimize the extraction conditions. Finally, a method of C₁₈IL in-tube SPME hyphen gas chromatography was established for the determination of PAHs in water. The limits of detection(LODs, S/N=3) were between 0.007 and 0.072 μg/L, and the limits of quantification(LOQs, S/N=10) varied from 0.023 to 0.24 μg/L. The intra- and inter-day relative standard deviations(RSDs) of the PAHs were below 10% except for that of phenanthrene. The proposed method was also applied to the determination of the PAHs in a coffee sample, and the recoveries for the five PHAs(spiked in the coffee sample at three levels) ranged from 85.79% to 103.42%.

Key words: Ionic liquid, Monolithic column, In-tube solid phase microextraction, Polycyclic aromatic hydrocarbons

CLC Number:

O657

TrendMD:

ZHANG Na, WAN Xin, SONG Xuyan, HUANG Long, ZHENG Jingjing, XING Jun. Application of Octadecyl Ionic Liquid Hybrid Solid-phase Microextraction Monolithic Column in the Detection of Polycyclic Aromatic Hydrocarbons in Coffee^†[J]. Chem. J. Chinese Universities, 2017, 38(6): 1033.

Figures/Tables 10

References 32

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PAHs	RSD(%)
PAHs	Repeatability(n=3)	Column-to-column repeatability(n=3)
Nap	10.1	12.2
Flu	7.4	7.9
Phe	6.9	7.2
FL	4.8	11.7
Pyr	4.9	9.4

PAHs	RSD(%)
PAHs	Repeatability(n=3)	Column-to-column repeatability(n=3)
Nap	10.1	12.2
Flu	7.4	7.9
Phe	6.9	7.2
FL	4.8	11.7
Pyr	4.9	9.4

PAHs	Linear range/ (μg·L^-1)	Linear regression			LOD/ (μg·L^-1)	LOQ/ (μg·L^-1)	RSD(%, n=5)
PAHs	Linear range/ (μg·L^-1)	Slope			Intercept	R²	Intra-day	Inter-day
Nap	0.4—200	605.28	1192.7	0.9998	0.072	0.240	7.9	9.6
Flu	0.1—200	1192.00	-152.13	0.9994	0.016	0.053	6.3	9.7
Phe	0.1—200	1081.40	480.43	0.9997	0.008	0.027	5.3	12.6
FL	0.1—200	845.05	-424.32	0.9992	0.007	0.023	2.0	8.4
Pyr	0.1—200	770.26	120.27	0.9995	0.013	0.043	2.2	4.9

PAHs	Linear range/ (μg·L^-1)	Linear regression			LOD/ (μg·L^-1)	LOQ/ (μg·L^-1)	RSD(%, n=5)
PAHs	Linear range/ (μg·L^-1)	Slope			Intercept	R²	Intra-day	Inter-day
Nap	0.4—200	605.28	1192.7	0.9998	0.072	0.240	7.9	9.6
Flu	0.1—200	1192.00	-152.13	0.9994	0.016	0.053	6.3	9.7
Phe	0.1—200	1081.40	480.43	0.9997	0.008	0.027	5.3	12.6
FL	0.1—200	845.05	-424.32	0.9992	0.007	0.023	2.0	8.4
Pyr	0.1—200	770.26	120.27	0.9995	0.013	0.043	2.2	4.9

Method	Sample	LOD/(μg·L^-1)						Ref.
Method	Sample	Nap		Flu	Phe	FL	Pyr	Nap
C₁₈IL in-tube SPME(10 cm)-GC-FID	Coffee	0.072	0.016	0.008	0.007	0.013	0.072	This work
LDS-DLLME^a-GC-MS	Water	0.058	0.023	0.028	0.038	0.037	0.058	[27]
Polyester fibers-in-tube(30 cm) SPME-HPLC-DAD	Water	0.01	0.01	0.01	0.03	0.01	0.01	[28]
Poly(SAM-DVB) monolithic(50 cm)-CEC-APCI-MS	Seafood		26.7		2.7	1.1		[29]
MSPE^b-HPLC-FLD	Coffee and tea			0.005				[30]
Si-MWCNTs monolithic(3 cm)-SPME-GC-MS	Water	0.1		0.1	0.1	0.1	0.1	[31]