Vol.:(0123456789) 1 3
J IRAN CHEM SOC (2017) 14:2665–2671
DOI 10.1007/s13738-017-1201-2
ORIGINAL PAPER
Determination of trace amounts of nystatin in water and vaccine
samples using sodium dodecyl sulfate‑coated iron oxide
magnetic nanoparticles followed by high‑performance liquid
chromatography–ultraviolet detection
Marjan Hematyar
1
· Ali Es‑haghi
2
· Majid Soleimani
1
· Ali Rezaie Mokarram
3
Received: 22 March 2017 / Accepted: 12 September 2017 / Published online: 3 October 2017
© Iranian Chemical Society 2017
50, 300 and 500 µg L
−1
) for water and vaccine samples,
respectively.
Keywords Magnetic solid-phase extraction · Mixed
hemi/ad-micelles · Nystatin · Vaccine
Abbreviations
MNPs Magnetic nanoparticles
MSPE Magnetic solid-phase extraction
NYS Nystatin
SDS Sodium dodecyl sulfate
HPLC/UV High-performance liquid chromatography–
ultraviolet detection
LC–MS Liquid chromatography–mass spectrometry
CE Capillary electrophoresis
HPTLC High-performance thin layer chromatography
FESEM Field emission scanning electron microscope
FTIR Fourier transform infrared
RSD Relative standard deviation
LOD Limit of detection
LOQ Limit of quantifcation
FMD Foot and mouth disease
Introduction
The addition of preservatives to vaccine/biologic formula-
tions is allowed or, in case of multi-dose preparations, pre-
scribed in all pharmacopeias. These substances are added
in order to kill or to inhibit the growth of harmful bacteria
and fungi which introduced unintentionally at any stage of
manufacturing process or at any time during use and storage.
Therefore, regular control is necessary: as it gives assurance
that the biological products have been adequately preserved
Abstract In this work, magnetic solid-phase extraction
based on sodium dodecyl sulfate-coated Fe
3
O
4
nanoparti-
cles has been successfully applied for extraction and pre-
concentration of trace amounts of nystatin from water and
vaccine samples prior to high-performance liquid chroma-
tography–ultraviolet detection. Various experimental param-
eters afecting extraction and recovery of the analyte, such
as the amount of sodium dodecyl sulfate, pH of the sample
solution, salt concentration, extraction time, sample volume
and desorption conditions, were systematically studied and
optimized. Under optimized conditions, nystatin was quan-
titatively extracted. Proper linear range with good coef-
cient of determination, (R
2
> 0.99) and limit of detection and
quantifcation (based on signal-to-noise ratios of 3 and 10) of
2.0 and 5.0 µg L
−1
, over the investigated concentration range
(5–700 µg L
−1
), were obtained, respectively. The intra-day
and inter-day relative standard deviations at 50 µg L
−1
level
of NYS were 1.4 and 4.5% based on six replicate determina-
tions. The accuracy of the method was evaluated by recov-
ery measurements on spiked samples. Suitable recoveries
of 96–102 and 26–44% were achieved (at spiked levels of
* Ali Es-haghi
a.eshaghi@rvsri.ac.ir
* Majid Soleimani
m-soleimani@hotmail.com
1
Department of Chemistry, Imam Khomeini International
University (IKIU), P.O. Box 288, Qazvin 34149-16818, Iran
2
Department of Physico Chemistry, Razi Vaccine and Serum
Research Institute, Agricultural Research, Education
and Extension Organization (AREEO), P.O. Box 31975/148,
Karaj, Iran
3
Department of QA, Razi Vaccine and Serum Research
Institute, Agricultural Research, Education and Extension
Organization (AREEO), P.O. Box 31975/148, Karaj, Iran