Malaysian
Journal of Analytical Sciences Vol 24 No 3
(2020): 373 - 381
HEADSPACE
MEMBRANE-PROTECTED LIQUID
PHASE MICROEXTRACTION OF
PHENANTHRENE IN BEVERAGE AND WATER
(Pengekstrakan Mikro Fasa Cecair Dilindungi Membran
Ruang Kepala bagi Fenantrena dalam Air Minuman dan Air)
Nor Hafiza Hassan, Wan
Mohd Afiq Wan Mohd Khalik, Saw Hong Loh*
Faculty
of Science and Marine Environment,
Universiti
Malaysia Terengganu, 21030 Kuala Nerus, Terengganu, Malaysia
*Corresponding
author: lohsh@umt.edu.my
Received: 30 March 2020;
Accepted: 29 April 2020; Published: 9 June
2020
Abstract
Contamination of low
molecular weights polycyclic aromatic hydrocarbons (PAHs) is common in beverage
and water. This could pose a health risk to those beverage lovers when they
consume the products. Phenanthrene (PHE) is one of the low molecular weights
PAHs that consists of three benzene rings in the molecular structure. In this
study, PHE was chosen as the model analyte due to its mid-volatility behavior.
A headspace membrane-protected liquid phase microextraction (HS-MP-LPME)
combined with high performance liquid chromatography-fluorescence detection
(HPLC-FD) has been developed for the analysis of PHE in beverage and water
samples. The nylon membrane containing 1-octanol as the extractant was exposed
to the headspace of the sample vial containing 25 mL of sample solution. The
extraction was performed at its optimal conditions with sample temperature
fixed at 60 °C, agitation set at 700 rpm and extraction conducted for 30 minutes.
Under these optimal extraction conditions, the HS-MP-LPME-HPLC-FD offered
ultra-trace detection of PHE and insignificant matrix effects in beverages
(green tea and coffee) and water (river, sea and tap) samples with average of
relative recovery in the range of 83.7 to 116.1%. The HS-MP-LPME simplifies the
routine analysis and resolves the extractant dissolution problem that commonly
occurs in hollow fiber-protected LPME. The proposed technique consumes only
minimal amounts of organic solvent (200 µL) and this indirectly supports our
National Green Technology Policy: together we create a better tomorrow.
Keywords: beverage,
water, headspace membrane-protected liquid phase microextraction, high
performance liquid chromatography-fluorescence, phenanthrene
Abstrak
Kontaminasi hidrokarbons aromatik polisiklik (PAHs) berjisim molekul
rendah dalam air minuman dan air adalah biasa. Ini akan menghasilkan risiko
kesihatan kepada pencinta air minuman apabila mereka minum produk tersebut.
Fenantrena (PHE) ialah salah satu PAHs berjisim molekul rendah yang mengandungi
tiga cincin benzena dalam struktur molekulnya. Dalam kajian ini, PHE dipilih
sebagai sebagai analit model kerana kemeruapannya yang sederhana. Satu
pengekstrakan mikro fasa cecair dilindungi membran ruang kepala (HS-MP-LPME) bergabung
dengan kromatografi cecair berprestasi tinggi-pengesanan pendarfluor (HPLC-FD) telah
dibangunkan untuk menganalisis PHE dalam sampel air minuman dan air. Membran
nilon yang mengandungi 1-oktanol sebagai pengekstrak didedahkan pada ruang
depan botol sampel yang berisi 25 mL larutan sampel. Pengekstrakan dilaksanakan
menggunakan keadaan optimum iaitu menetapkan suhu sampel pada 60 °C, mengacau
sampel pada kelajuan pengocakan 700 rpm dan mengekstrak selama 30 minit. Di
bawah keadaan pengekstrakan optimum, HS-MP-LPME-HPLC-FD menawarkan pengesanan
PHE pada tahap ultra-surihan dan memberi kesan matriks yang tidak signifikan
dalam sampel air minuman (tea hijau dan kopi) dan air (sungai, laut dan paip) dengan
perolehan semula secara relatif dalam lingkungan 83.7 hingga 116.1%. HS-MP-LPME
memudahkan analisis rutin dan menyelesaikan masalah pelarutan pengekstrak yang
biasa berlaku dalam LPME dilindungi fiber berongga. Teknik yang dicadangkan
hanya menggunakan kuantiti pelarut organik yang minimum dan ini menyokong
Polisi Hijau Nasional kita secara tidak langsung: bersama-sama kita membina
keesokan yang lebih baik.
Kata kunci: air minuman, air, pengekstrakan mikro
fasa cecair dilindungi membran pada ruang kepala, kromatografi cecair berprestasi
tinggi-pendarfluor, fenantrena
References
1.
Ramesh, A., Archibong,
A., Hood, D., Guo, Z. and Loganathan, B. (2011). Global environmental
distribution and human health effects of polycyclic aromatic hydrocarbons. Global Contamination Trends of Persistent
Organic Chemicals: pp. 97-126.
2.
Liu, H. and Dasgupta,
P. L. (1996). Analytical chemistry in a drop. solvent extraction in a microdrop.
Analytical Chemistry, 68(11):
1817-1821.
3.
Jeannot, M. A. and
Cantwell, F. F. (1996). Solvent microextraction into a single drop. Analytical Chemistry, 68(13): 2236-2240.
4.
Thordarson, E., Pálmarsdóttir,
S., Mathiasson, L. and Jönsson, J. A. (1996). Sample preparation using a miniaturized supported liquid
membrane device connected on-line to packed capillary liquid chromatography. Analytical Chemistry, 68(15): 2559-2563.
5.
Pedersen-Bjergaard, S.
and Rasmussen, K. E. (1999). Liquid−liquid−liquid
microextraction for sample preparation of biological fluids prior to capillary
electrophoresis. Analytical
Chemistry, 71(14): 2650-2656.
6. Wang,
J., Huang, S., Wang,
P. and Yang,
Y. (2016). Method
development for the analysis of phthalate esters in tea beverages by ionic
liquid hollow fibre liquid-phase microextraction and liquid chromatographic detection.
Food Control, 67: 278-284.
7.
Ali, W., Arain, M. B., Yamini, Y., Shah, N., Gul Kazi, T., Pedersen-Bjergaard, S. and Tajik,
M. (2019). Hollow fiber-based liquid
phase microextraction followed by analytical 2 instrumental techniques for
quantitative analysis of heavy metal ions and 3 pharmaceuticals. Journal of
Pharmaceutical Analysis, In press.
8.
Peng, J. F., Liu, R.,
Liu, J. F., He, B., Hu, X. L. and Jiang, G. B. (2007). Ultrasensitive determination of
cadmium in seawater by hollow fiber supported liquid membrane extraction
coupled with graphite furnace atomic absorption spectrometry. Spectrochimica Acta Part B: Atomic
Spectroscopy, 62(5): 499-503.
9. Sanagi,
M. M., Loh, S. H., Wan Ibrahim, W. A. and Hasan, M. N. (2012). Agarose film
liquid phase microextraction combined with gas chromatography–mass spectrometry
for the determination of polycyclic aromatic hydrocarbons in water. Journal of Chromatography A, 1262:
43-48.
10. Loh,
S. H., Sanagi, M. M., Wan Ibrahim, W. A. and Hasan, M. N. (2013). Solvent-impregnated
agarose gel liquid phase microextraction of polycyclic aromatic hydrocarbons in
water. Journal of Chromatography A,
1302: 14-19.
11. Chong,
Y. T., Mohd Ariffin, M., Mohd Tahir, N. and Loh, S. H. (2018). A green solvent
holder in electro-mediated microextraction for the extraction of phenols in
water. Talanta, 176: 558-564.
12. Sedehi,
S., Tabani, H. and Nojavan, S. (2018). Electro-driven extraction of polar compounds
using agarose gel as a new membrane: determination of amino acids in fruit
juice and human plasma samples. Talanta,
179: 318-325.
13. Sanagi,
M. M., See, H. H., Wan Ibrahim, W. A. and Abu Naim, A. (2007). Determination of
pesticides in water by cone shaped membrane protected liquid phase
microextraction prior to micro-liquid chromatography. Journal of Chromatography A, 1152: 215-219.
14.
Loh, T. Y., Khalik, W.
M. A. W. M. and Loh, S. H. (2020). Simple extraction of bisphenol A in
beverages and water by membrane-protected liquid phase microextraction. Sains Malaysiana, 49(1): 49-55.
15. Goh,
S. X. L., Goh, H. A. and Lee, H. K. (2018). Automation of ionic liquid enhanced
membrane bag-assisted-liquid-phase microextraction with liquid
chromatography-tandem mass spectrometry for determination of glucocorticoids in
water. Analytica Chimica Acta, 1035:
77-86.
16. Xu,
L. and Lee, H. K. (2009). Solvent-bar microextraction - using a silica monolith as
the extractant phase holder. Journal of
Chromatography A, 1216: 5483-5488.
17.
Ng, N. T., Sanagi, M.
M., Wan Ibrahim, W. N. and Wan Ibrahim, W. A. (2017). Agarose-chitosan-C18
film micro-solid phase extraction combined with high performance liquid
chromatography for the determination of phenanthrene and pyrene in
chrysanthemum tea samples. Food Chemistry,
222: 28-34.
18.
Kumar, B., Verma, V.
K., Gaur, R., Kumar, S., Sharma, C. S. and Akolkar, A. B. (2014). Validation of
HPLC method for determination of priority polycyclic aromatic hydrocarbons (PAHs)
in wastewater and sediments. Advances in
Applied Science Research, 5 (1): 201-209.
19.
Thorvaldsson, K. and
Janestad, H. (1999). A model for simultaneous heat, water and vapour diffusion.
Journal of Food Engineering, 40(3):
167-172.
20.
Vial, J. and Jardy, A.
(1999). Experimental comparison of the different approaches to estimate LOD and
LOQ of an HPLC method. Analytical
Chemistry, 71(14): 2672-2677.
21. Verbruggen,
E. M. J. and van Herwijnen, R. (2011). Environmental risk limits for
phenanthrene. National Institute for Public Health and the Environment, Ministry
of Health, Welfare and Sport, Netherlands.
22.
Loh, S. H., Chong, Y.
T., Nor Afindi, K. N. and Abdullah Kamaruddin, N. (2016). Determination of
Polycyclic aromatic hydrocarbons in beverage by low density solvent
based-dispersive liquid-liquid microextraction-high performance liquid
chromatography-fluorescence detection. Sains
Malaysiana, 45 (10): 1453-1459.
23.
Loh, S. H., Neoh, P.
E., Tai, C. T. and Kamaruzaman, S. (2018). Simple µ-solid phase extraction
using C18 film for the extraction of polycyclic aromatic
hydrocarbons in coffee beverage. Malaysian
Journal of Analytical Sciences, 22(1): 1-7.
24.
Shi, Y., Wu, H., Wang,
C., Guo, X., Du, J. and Du, L. (2016). Determination of polycyclic aromatic
hydrocarbons in coffee and tea samples by magnetic solid-phase extraction
coupled with HPLC–FLD. Food Chemistry,
199: 75- 80.