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The Acute Toxicity Test of Methanolic Extract of Hyptis pectinata Poit on LiverBalb/c Mice (Conference Paper) (Open Access)

, ,

Department of Chemistry, Faculty of Science and Mathematics, Diponegoro University, Semarang, IndonesiaPhysiology and Microanatomy Division, Faculty of Veterinary Medicine, Gadjah Mada University, Jogjakarta,

Indonesia

AbstractPlants from Lamiaceae family has almost entirely reported having physiological activities. One of them is Hyptispectinata Poit plant. Research on the toxicity of Hyptis pectinata needs to be done to protect people from thepossibility of its harmful effects. This study aim to know the acute toxicity effects of Hyptis pectinata extract (HPE) onliver of Balb/c mice. This research was a laboratory experimental study using the post test only controlled groupdesign. Balb/c mice were randomly divided into 4 groups. K (control group), P1, P2 and P3 (treatment groups; givenHPE 200mg/kgBW, 1000 mg/kgBW, and 5000 mg/kgBW, respectively). The extract was orally given with gastric tubeon the first day and the mice were terminated at the 8th day then the livers were observed. The Kruskal-Wallis test formacroscopic morphological and volume of the liver showed there were no significant difference with p=0.406 andp=0.054. The highest liver histopathological score was in P3 group. The Kruskal-Wallis test showed significantlydifference (p=0.000). Continued with Mann-Withney test that showed a significant difference in K-P1 (p=0.009), K-P2(p=0.009), K-P3 (p=0.009), P1-P2 (p=0.028), and P1-P3 (p=0.009). In conclusion, the HPE is safe to use which has nocomplication with liver of mice. © Published under licence by IOP Publishing Ltd.

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Indexed keywords

Engineeringcontrolled terms:

Testing Toxicity

Engineeringuncontrolled terms

Acute toxicity test Control groups Harmful effects Kruskal-Wallis tests Lamiaceae family

Methanolic extracts Physiological activity Treatment group

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Mammals

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IOP Conference Series: Materials Science and EngineeringVolume 172, Issue 1, 17 February 2017, Article number 01202911th Joint Conference on Chemistry, JCC 2016, in Conjunction with the 4th RegionalBiomaterials Scientific Meeting; Purwokerto; Indonesia; 15 September 2016 through 16September 2016; Code 126603

Suzery, M.a Cahyono, B.a Astuti, P.b

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Hyptis | Oils, Volatile | Gastric ulcer

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ISSN: 17578981Source Type: Conference ProceedingOriginal language: English

DOI: 10.1088/1757-899X/172/1/012029Document Type: Conference PaperSponsors:Publisher: Institute of Physics Publishing

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Antinociceptive and antiedematogenic effects of the aqueous extract of Hyptispectinata leaves in experimental animals

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α-Pyrones and a 2(5H)-furanone from Hyptis pectinata

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The essential oil of Hyptis pectinata.

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Screening for antimicrobial activity of crude drug extracts and pure natural productsfrom Mexican medicinal plants

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Melo, G.B., Silva, R.L., Melo, V.A., Antoniolli, Â.R., Jordani Souza, M.E., Jordani, M.C., Castro-e-Silva Jr., O.

(2005) Phytomedicine, 12 (5), pp. 359-362.  .

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Darmansjah, I., Wiria, M.S.S.(2007) Farmakologi Dan Terapi, pp. 820-825.Darmansjah I and Wiria MSS 5 ed SG Gunawan, R Setiabudy and Elysabeth Nafrialdi (Jakarta: DepartemenFarmakologi dan Terapeutik Fakultas Kedokteran Universitas Indonesia) Dasar Toksikologi

 

Robins, S.L., Kumar, V.(1995) , 3, p. 18.Robins SL and Kumar V 4 ed Alih bahasa and BU Pendit (Jakarta: EGC) Buku Ajar Patologi II

 

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Suzery, M., Cahyono, B.Evaluation of Cytotoxicity Effect of Hyptis pectinata Poit (Lamiaceae) extracts using BSLT and MTT methods(2014) Jurnal Sains Dan Matematika, 22, pp. 82-86.  .

 

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Effect of the aqueous extract of Hyptis pectinata on liver mitochondrial respiration

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IOP Conference Series: Materials Science and EngineeringScopus coverage years: from 2009 to 2019ISSN: 1757-8981 E-ISSN: 1757-899XSubject area: Engineering: General Engineering Materials Science: General Materials Science

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JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 011001 doi:10.1088/1757-899X/172/1/011001

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Committee

Chairman : Amin Fatoni, Ph.D (Universitas Jenderal Soedirman, Indonesia)

Secretary : Anung Riapanitra, M.Sc. (Universitas Jenderal Soedirman, Indonesia)

Dr. Hartiwi Diastuti (Universitas Jenderal Soedirman, Indonesia)

Treasurer : Senny W, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Dian Riana N, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Dian Windy Dwiasi, M.Sc. (Universitas Jenderal Soedirman, Indonesia)

Moch. Chasani, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Kapti Riyani, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Scientific : Uyi Sulaiman, Ph.D. (Universitas Jenderal Soedirman, Indonesia)

Dadan Hermawan, Ph.D. (Universitas Jenderal Soedirman, Indonesia)

Dr. Suwandri (Universitas Jenderal Soedirman, Indonesia)

Puji Lestari, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Mardiyah K, M.Sc. (Universitas Jenderal Soedirman, Indonesia)

Zusfahair, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Program : Ari Asnani, Ph.D. (Universitas Jenderal Soedirman, Indonesia)

Dr. Ponco Iswanto (Universitas Jenderal Soedirman, Indonesia)

Roy Andreas, Ph.D. (Universitas Jenderal Soedirman, Indonesia)

Suyata, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Tien Setyaningtyas, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Eva Vaulina, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Purwati, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Publication : Dwi Kartika, M.Sc. (Universitas Jenderal Soedirman, Indonesia)

Ely Setiawan, M.Si. (Universitas Jenderal Soedirman, Indonesia)

Irmanto, M.Si. (Universitas Jenderal Soedirman, Indonesia)

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 011001 doi:10.1088/1757-899X/172/1/011001

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International Scientific Board

1. Prof. Dr. Hadi Nur (Universiti Teknologi Malaysia) 2. Prof. Dr. Hassan Y. Aboul-Enein (National Research Centre, Cairo, Egypt) 3. Prof. Dr. Ahmad Zuhairi Abdullah (Universiti Sains Malaysia, Malaysia) 4. Assoc. Prof. Dr. Panote Thavarungkul (Prince of Songkla University, Thailand) 5. Assoc. Prof. Dr. J. Yan Mulyana (Tokyo Metropolitan University, Japan) 6. Dr. Oki Muraza (King Fahd University of Petroleum and Minerals, Saudi Arabia) 7. Assoc. Prof. Dr. Imran Parvez (Hajee Mohammad Danesh Science and

Technology University (HSTU), Bangladesh) 8. Dr. Danjuma Solomon (Ibrahim Badamasi Babangida University, Nigeria) 9. Uyi Sulaiman, Ph.D (Universitas Jenderal Soedirman, Indonesia) 10. Dr. Dwi Hudiyanti, M.Sc (Diponegoro University, Indonesia) 11. Dr. Khairul Anam (Diponegoro University, Indonesia) 12. Ismiyarto, Ph.D (Diponegoro University, Indonesia) 13. Adi Darmawan, Ph.D (Diponegoro University, Indonesia) 14. Dr. rer.nat Maulidan Firdaus, M.Sc (Sebelas Maret University, Indonesia) 15. Venty Suryanti, Ph.D (Sebelas Maret University, Indonesia) 16. Dr. Eddy Heraldy (Sebelas Maret University, Indonesia) 17. Dr.rer.nat. Witri Wahyu Lestari (Sebelas Maret University, Indonesia) 18. Dr. Dian M. Widjonarko, M.Si (Sebelas Maret University, Indonesia) 19. Dr. Hartati Soetjipto (Satyawacana Christian University, Indonesia) 20. Ir. Sri Hartini, M.Sc (Satyawacana Christian University, Indonesia) 21. Dr. Risfidian Mohadi (Sriwijaya University, Indonesia) 22. Dr. Mokosuli Yermia S (Manado State University, Indonesia)

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 011001 doi:10.1088/1757-899X/172/1/011001

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4/7/2020 IOP Conference Series: Materials Science and Engineering, Volume 172, 2017 - IOPscience

https://iopscience.iop.org/issue/1757-899X/172/1 1/11

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Volume 1722017

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11th Joint Conference on Chemistry in Conjunction with the 4th Regional BiomaterialsScientific Meeting 15–16 September 2016, Purwokerto, Indonesia

Accepted papers received: 25 January 2017Published online: 17 February 2017

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4/7/2020 IOP Conference Series: Materials Science and Engineering, Volume 172, 2017 - IOPscience

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4/7/2020 IOP Conference Series: Materials Science and Engineering, Volume 172, 2017 - IOPscience

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The Acute Toxicity Test of Methanolic Extract of Hyptis pectinata Poit on Liver Balb/c MiceM Suzery, B Cahyono and P Astuti

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The Acute Toxicity Test of Methanolic Extract of Hyptis

pectinata Poit on Liver Balb/c Mice

M Suzery1, B Cahyono1 and P Astuti2 1Department of chemistry, Faculty of Science and Mathematics Diponegoro University,

Semarang, Indonesia 2Physiology and Microanatomy Division, Faculty of Veterinary Medicine, Gadjah Mada

University, Jogjakarta, Indonesia

Email: [email protected]

Abstract. Plants from Lamiaceae family has almost entirely reported having physiological

activities. One of them is Hyptis pectinata Poit plant. Research on the toxicity of Hyptis

pectinata needs to be done to protect people from the possibility of its harmful effects. This

study aim to know the acute toxicity effects of Hyptis pectinata extract (HPE) on liver of

Balb/c mice. This research was a laboratory experimental study using the post test only

controlled group design. Balb/c mice were randomly divided into 4 groups. K (control group),

P1, P2 and P3 (treatment groups; given HPE 200mg/kgBW, 1000 mg/kgBW, and 5000

mg/kgBW, respectively). The extract was orally given with gastric tube on the first day and the

mice were terminated at the 8th day then the livers were observed. The Kruskal-Wallis test for

macroscopic morphological and volume of the liver showed there were no significant

difference with p=0.406 and p=0.054. The highest liver histopathological score was in P3

group. The Kruskal-Wallis test showed significantly difference (p=0.000). Continued with

Mann-Withney test that showed a significant difference in K-P1 (p=0.009), K-P2 (p=0.009),

K-P3 (p=0.009), P1-P2 (p=0.028), and P1-P3 (p=0.009). In conclusion, the HPE is safe to use

which has no complication with liver of mice.

1. Introduction

There are at least 295 genera and 7775 species of plants from Lamiaceae family and most widely

found in Mexico, Senegal, Brazil, Spain and in Asia such as India, Malaysia and Indonesia. Some

species of this genus of plants, namely Hyptis pectinata Poit, Hyptis suaveolens, Hyptis oblingofolia,

Hyptis tumentosa, Hyptis verticillata, Hyptis capitata, Hyptis brevives Poit, Hyptis fruktikosa and

Hyptis urticoide, almost entirely reported to have physiological activities. The activities shown by this

plant: anti-inflammatory, antipyretic, cancer [1, 2], ease breathing, skin diseases [3], disorders of the

stomach, fever [4], and infections by bacteria [5].

In India, Hyptis pectinata Poit leaves are made in the form of tea which used as a beverage prevent

abdominal pain [2]. Water extract of this plant has also been reported to increase liver regeneration

[6].

Currently, in society the issue back to nature is growing and thus influence use of traditional

medicine tends to increase. Meanwhile, many people assume that the use of herbs or traditional

medicines are relatively safer than synthetic drugs. However it does not mean herbs or traditional

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012029 doi:10.1088/1757-899X/172/1/012029

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

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Interlayer free – nickel doped silica membranes for

desalination

A Darmawan1,*

, L Karlina1, Y Astuti

1, Sriatun

1, D K Wang

2, J Motuzas

2, J C D

da Costa2

1Diponegoro University, Department of Chemistry, Semarang 50275, Indonesia.

2The University of Queensland, FIM2Lab-Functional Interfacial Materials and Membranes

Laboratory, School of Chemical Engineering, Brisbane Qld 4072, Australia.

*corresponding author e-mail: [email protected]

Tel.:+62-8222-121-9817

Abstract. This work shows for the first time the potential of nickel oxide silica membranes for

desalination applications. Nickel oxide silica xerogels were synthesised via a sol–gel method

including TEOS, nickel nitrate with and without addition of hydrogen peroxide. The effects of

nickel addition (5% - 50 mol %) on the structure–property relationship of the silica materials

were systematically studied. The membrane performance were tested as a function of feed salt

concentration (0.3–3.5 wt% NaCl) and temperature (27–60 °C). The membranes which were

prepared using equal sol–gel conditions to the xerogel samples showed the raised feed

temperatures resulted in increased water fluxes, whilst increasing the salt concentration

resulted in decreased water fluxes. The membranes with addition of hydrogen peroxide

exhibited better performances than their H2O2 absence counterpart. The salt rejection was in

excess of 90% and the maximum flux observed was 7.3 kg m-2

h-1

at 60°C for a 0.3 wt% NaCl

feed concentration.

Introduction

The world is facing a global water crisis due to population growth and climate change [1]. With

increasingly limited water resources, the use of infinite number of sea water becomes one choice in the

provision of clean and fresh water, hence the desalination technology is one of solution[2]. Currently,

approximately 43.5% of the desalination systems in the world are still using thermal technology.

Membrane technology becomes an alternative instead of thermal desalination [3] because it uses less

energy and produce greater water fluxes. In commercial applications, the polymeric membrane are still

dominating the market despite of the polymeric membranes have some limitations, especially in their

thermal and chemical stability, hence some researchers tried to find a new alternative using inorganic

membranes [4-10]

There are two types of inorganic membranes that have been tested for molecular sieve application,

zeolite membranes and silica membranes. In general, silica membranes are developed primarily for

gas separation [11, 12]. However, some studies have shown that silica membranes coated on alumina

support could reject salt ranging from 92% to 99% [8, 10, 13-15]. However, one of the main obstacles

in using silica membranes for water purification is due to their hydro instability. To overcome this

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012001 doi:10.1088/1757-899X/172/1/012001

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd

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Development of high performance liquid chromatography

method for miconazole analysis in powder sample

D Hermawan1, Suwandri

1, U Sulaeman

1, A Istiqomah

1 and H Y Aboul-Enein

2

1 Department of Chemistry, Faculty of Mathematics and Natural Sciences, Jenderal Soedirman

University, Purwokerto, Indonesia 2

Department of Pharmaceutical and Medicinal Chemistry, Pharmaceutical and Drug Industries

Research Division, National Research Centre, Dokki, Cairo, Egypt

Email: [email protected]

Abstract. A simple high performance liquid chromatography (HPLC) method has been

developed in this study for the analysis of miconazole, an antifungal drug, in powder sample.

The optimized HPLC system using C8 column was achieved using mobile phase composition

containing methanol:water (85:15, v/v), a flow rate of 0.8 mL/min, and UV detection at 220

nm. The calibration graph was linear in the range from 10 to 50 mg/L with r2 of 0.9983. The

limit of detection (LOD) and limit of quantitation (LOQ) obtained were 2.24 mg/L and 7.47

mg/L, respectively. The present HPLC method is applicable for the determination of

miconazole in the powder sample with a recovery of 101.28 % (RSD = 0.96%, n = 3). The

developed HPLC method provides short analysis time, high reproducibility and high

sensitivity.

1. Introduction

Many types of drugs are produced synthetically and commercially available in dosage forms. One

example of important drugs used as a medication is antifungal drugs. An antifungal drug is used to

treat deep infections caused by a fungus. This drug can be divided into several classes, including

triazoles and imidazoles. Miconazole is an imidazole antifungal agent (figure 1). It is commonly used

to the skin or to mucous membrane to cure fungal infections, due to its high therapeutic properties. It

has been extensively applied in the management of dermal, oral and vaginal mycosis. It is used in a

variety of pharmaceutical formulations such as injections, tablets, oral gels, creams, ointments, topical

powders and vaginal suppositories. The most usual application forms include creams, ointments or gels

at 2.0 % concentration level, alone or associated with anti-inflammatory steroids, or other

antimicrobials such as gentamicin for the treatment of dermatitis. Diaper dermatitis, a common

dermatologic disorder in infancy, frequently associated with Candida albicans infections, is currently

treated with ointments containing 0.25 % miconazole nitrate [1-2].

Chromatographic methods have achieved a great reputation in separation science; mainly using

high performance liquid chromatography (HPLC) method [3-10]. The chromatographic process can be

described as a separation technique that includes mass-transfer between stationary and mobile phase.

HPLC uses a liquid mobile phase to separate the components in a mixture. The stationary phase can be

in a liquid phase or a solid phase. These components are forced to flow through a chromatographic

column under high pressure after being dissolved in a solvent. The mixture is then separated into its

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012011 doi:10.1088/1757-899X/172/1/012011

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd

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Surface modifications of chalcopyrite CuInS2 thin films for

photochatodes in photoelectrochemical water splitting under

sunlight irradiation

Gunawan,1 A Haris,

1 H Widiyandari,

2 W Septina

3 and S Ikeda,

4

1Chemistry Department, Faculty of Sciences and Mathematics, Diponegoro University,

Semarang Indonesia 2Physics Department, Faculty of Sciences and Mathematics, Diponegoro University, Semarang

Indonesia 3University of Zurich, Switzerland

4Konan University, Osaka, Japan

E-mail: [email protected]

Abstract. Copper chalcopyrite semiconductors include a wide range of compounds that are of

interest for photoelectrochemical water splitting which enables them to be used as

photochatodes for H2 generation. Among them, CuInS2 is one of the most important materials

due to its optimum band gap energy for sunlight absorption. In the present study, we

investigated the application of CuInS2 fabricated by electrodeposition as photochatodes for

water splitting. Thin film of CuInS2 chalcopyrite was formed on Mo-coated glass substrate by

stacked electrodeposition of copper and indium followed by sulfurization under H2S flow. The

films worked as a H2 liberation electrode under cathodic polarization from a solution

containing Na2SO4 after loading Pt deposits on the film. Introduction of an n-type CdS layer by

chemical bath deposition on the CuInS2 surface before the Pt loading resulted appreciable

improvements of H2 liberation efficiency and a higher photocurrent onset potential. Moreover,

the use of In2S3 layer as an alternative n-type layer to the CdS significantly improved the H2

liberation performance: the CuInS2 film modified with In2S3 and Pt deposits worked as an

efficient photocathode for photoelectrochemical water splitting.

1. Introduction

The shortage of fossile sources has made an effort to get alternative energies such as hydrogen through

its conversion to energy by direct combustion in conventional engines or reaction with pure oxygen in

a fuel cell. Hydrogen can be produced by natural gas reforming, electrolysis, biomass, thermochemical,

thermophysical, photoelectrochemical (PEC) methods, and photo-biological process [1]. Hydrogen

(H2) production by PEC water splitting is considered to be an attractive in view of energy and

environmental issues.

Since the first report of a TiO2 thin-film photoelectrode [2], a variety of semiconductor electrodes

and devices have been investigated. To date, performances with conversion efficiency as high as

12.4% have been demonstrated for electrodes based p-GaInP2/GaAs cells grown by atmospheric-

pressure organometallic vapor-phase epitaxy [3]. However, due to limited corrosion resistance in

aqueous electrolytes and expensive cost for production of these electrodes, these systems are not

feasible for practical applications. Meanwhile, corrosion-resistant and inexpensive transition metal

oxides are well-studied, but conversion efficiencies for these electrodes are not sufficiently high yet

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012021 doi:10.1088/1757-899X/172/1/012021

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd

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Unsaturated 15 and 16 Membered Appended Naphthalene

Macrocyclic Molecules for The Development of Fluorometric

Chemosensors

S Hasan1 ,S Salleh 1, S Hamdan1 , and B Yamin1

1Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam,

Selangor, Malaysia.

e-mail:[email protected]

Abstract. Unsaturated macrocyclic molecules have got an interest due to their potential in

catalysis, ion exchange and electron transfer. Salicaldehyde derivatives macrocyclic molecules

have a broad range in synthesis. In this study, two unsaturated macrocyclic molecules (L1 and

L2) have been synthesized. The preparation of unsaturated macrocyclic ligands involve two

steps; the reaction of salicylaldehyde with 1,2-dibromoethane or 1,4-dibromobutane to produce

precursor, then cyclisation were completed using schiff base technique by adding diamines

(naphthalene diamine). The ligands were characterized spectroscopically. In FT-IR spectrums,

the form of the ligands mainly can be observed on the disappearance of the carbonyl group of

aldehyde at approximately 1650cm-1 that was readily assigned to C=O group of salicylaldehyde

with the replacement of C=N peak at 1684.13cm-1. The success in producing macrocyclic

ligands have been further characterized using fluorescence emission spectroscopy (FES) and

revealed the typical emission of naphthalene at ~430nm. Fluorescence changes of L1 and L2

showed high selectivity for Fe3+ and Cu2+ respectively in the presence of other common metal

ions, such as Zn2+, Ni2+ and Co2+. Besides, the ligand was sensitive enough to detect the

concentration of ferric ion with the detection limit down to 1.08 x 10-6 M and fluorescence

change that was unaffected by the presence of other common coexisting metal ions.

Complexation with Co(II) was also attempted.

Keywords: Macrocyclic Schiff base, Macrocyclic complexes. 1,2-bis(2-carboxyaldehyde

phenoxy)ethane, Cobalt(II)complexes,1,8- Naphthalenediamine, Fluorophore.

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012054 doi:10.1088/1757-899X/172/1/012054

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd

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Dimethylaminodiethylenetriamine Derivatives of Fluorescence

Chemosenso for Detection of Zn2+ In Aqueous Solution

S N A M Adnan1, S Hasan1, S Zakaria1 and Y M Yusof1

1Faculty of Applied Sciences Universiti Teknologi MARA 40450 Shah Alam, Selangor,

Malaysia

Email: [email protected]

Abstract. Fluorescent chemosensors for the detection and measurement of metal ions,

especially for cations environmental interest such as Fe3+, Co2+, Mn2+, Cu2+, and Zn2+ are

actively investigated because it shows simplicity, high sensitivity and fast response. New

benzenyl derivative bearing pyridine group has been synthesized and studied as fluorescent

chemosensor for Zn2+ ion. Chemosensor N-{2-[(4-Dimethylamino-benzylidene)-amino]-

ethyl}-N'-pyridin-2-ylmethylene-ethane-1,2-diamine was synthesized by condensation of p-

dimethylaminobenzaldehyde, diethylenetriamine and o-pyridinecarbaldehyde and characterized

by FT-IR, 1H-NMR and elemental analysis (CHN). FT-IR showed the appearance of peak

azomethine (C=NH) at 1639.46 cm-1, pyridine (C-N) at 1591 cm-1and disappearance of NH2

peak at 3278.78 cm-1 after the condensation reaction in between aldehyde and amine. 1H-NMR

signal at 8.19 ppm, 3.12 ppm and 8.08 ppm was assigned to C=NH, N(CH3)2 and C-N

respectively, confirmed the formation of N-{2-[(4-Dimethylamino-benzylidene)-amino]-

ethyl}-N'-pyridin-2-ylmethylene-ethane-1,2-diamine. The elemental analysis was found closed

to the theoretical value and the percent composition of A is 91.82%. Sensor A exhibits high

selectivity and sensitivity towards Zn2+. Other metal ions such Cu2+, Fe3+, Co2+ and Ni2+ had no

such significant effect on the fluorescence. The detection limit of N-{2-[(4-Dimethylamino-

benzylidene)-amino]-ethyl}-N'-pyridin-2-ylmethylene-ethane-1,2-diamine for Zn2+ was 3.5 x

10-5 M. M. This sensor exhibits a very good fluorescence sensing ability to Zn2+ over a wide

range of pH. Therefore it is capable of being a practical system for the monitoring of Zn2+

concentrations in real water sample.

1. Introduction

Zinc is the second most abundant transition metal ion in the human body, it plays an indispensable

role in various biological activities such as gene expression, neural signal transmission, regulation of

metalloenzymes, and DNA binding or recognition [1]. However, excessive amounts of zinc in human

cause many severe diseases such as Alzheimer’s disease [2], ischemic stroke [3] and epilepsy [4].

Hence it is very important to develop highly selective and sensitive chemosensors for the detection of

Zn2+ in the environment as well as biological samples.

Owing to its essential roles in biological nutrition systems, the measurement of Zn2+ is an active

field in analytical chemistry. Compared with numerous traditional analytical techniques, fluorescence

molecule sensor display high sensitivity, selectivity, simplicity, and tunability thus have been

developed as a powerful tool for detecting the trace amount of analytes. Chemosensors are commonly

composed of two parts, a receptor (recognition element) responsible for the molecular recognition of

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012051 doi:10.1088/1757-899X/172/1/012051

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd

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Synthesis and characterization of p-

dimethylaminobenzaldehyde benzoylthiourea and study

towards selective and sensitive fluorescent sensor for detection

of iron (III) cation in aqueous solution.

S Hasan1, N A Hamedan1, A A A Razali1, N H Uyup1, and H M Zaki1

1Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor,

Malaysia.

Email: [email protected]

Abstract. Benzoyl thiourea derivatives ligand backbones contain Oxygen (O), Nitrogen (N),

and Suphur (S) donor atoms can react with transition metal ions and form stable metal

complexes. A new ligand was synthesized by the reaction of benzoyl isothiocyanate with

diethylenetriamine and characterized by using Elemental Analysis (EA), Infrared (IR)

spectroscopy and proton Nuclear Magnetic Resonance (1H NMR) spectroscopy. The

monofunctionalize ligand were synthesized using 1:1 condensation of p-

dimethylaminobenzaldehyde with diethylenetriamine and confirmed by disappearance of

carbonyl group, C=O at 1656 cm-1 with the appearance of peak C=N in the range 1633 - 1638

cm-1 in the IR spectrum. This monofunctionalize ligand was synthesis by using Schiff base

technique. Benzoyl thiourea derivatives, HN are synthesis from the 1:1 condensation of

benzoyl isothiocyanates with monofunctionalized ligand. HN ligand was verified by the

presence of peaks v(N-H), v(C=O), v(C=N) v(C-N) and v(C=S) at 3317 - 3336 cm-1, 1612 -

1660 cm-1, 1550 -1589 cm-1, 1234-1366 cm-1 and 709-767 cm-1 respectively while 1H NMR

show peaks of alkane (CH2), benzene (Ar-H), CONH, CSNH at 3.75, 6.73 – 7.33, 8.19, and

8.25 respectively. The total percent composition of C, H, N, O, and S using Elemental Analysis

for HN, C21H27N5OS found was 85.23%. For application, further study on selectivity and

sensitivity of HN ligand was conducted on several metal ions. The fluorescent emission

spectroscopy shown that HN is a selective fluorescent sensor for Fe3+ and Cu2+ ions but not for

other metal ions such as Co2+, Ni2+, Mn2+, Cr3+ and Zn2+. However, HN ligand shows more

sensitive towards Fe3+ ions than Cu2+ ions which provide rapid detection of Fe3+ ions at

concentrations as low as 4.5 x 10-7 M than 2.9 x 10-6 M of Cu2+ ions. As conclusion, HN ligand

was expected to be useful as efficient chemical sensor for detection of Fe3+ ion.

1. Introduction

Nowadays, the development of chemosensors for selectivity and sensitivity quantification of

environmentally and biologically for heavy and transition metal ions, has attracted a high attention [1].

They usually represent an environmental concern when present in uncontrolled amounts, but at the

same time some of them such as iron, zinc, manganese, copper and cobalt are present as essential

elements in biological systems. Among biologically important metal ions, iron is the most abundant

transition metal ion present in the human body. As one of the most essential trace elements in

1

JCC2016 IOP PublishingIOP Conf. Series: Materials Science and Engineering 172 (2017) 012050 doi:10.1088/1757-899X/172/1/012050

International Conference on Recent Trends in Physics 2016 (ICRTP2016) IOP PublishingJournal of Physics: Conference Series 755 (2016) 011001 doi:10.1088/1742-6596/755/1/011001

Content from this work may be used under the terms of the Creative Commons Attribution 3.0 licence. Any further distributionof this work must maintain attribution to the author(s) and the title of the work, journal citation and DOI.

Published under licence by IOP Publishing Ltd