Sains Malaysiana 44(1)(2015): 121–126
A
Thermal Degradation (Thermolysis) Study of Rotenone Extracted from Derris
elliptica Roots Using Reverse-Phase High Performance Liquid Chromatography
(RP-HPLC)
(Kajian Degradasi Terma (Termolisis)
bagi Rotenon dalam Cecair Ekstrak Mentah Pekat (CLCE)
Diekstrak daripada Akar Derris elliptica Menggunakan Fasa
Keterbalikan Cecair Kromatografi Berprestasi Tinggi (HPLC))
SAIFUL IRWAN ZUBAIRI1*, MOHAMAD ROJI SARMIDI2 & RAMLAN ABDUL AZIZ2
1School of Chemical
Sciences & Food Technology, Faculty of Science & Technology
Universiti Kebangsaan
Malaysia, 43600 Bangi, Selangor Darul Ehsan, Malaysia
2Institute of Bioproduct
Development, Universiti Teknologi Malaysiam 81310 Skudai,
Johor Darul Takzim, Malaysia
Received: 20 August
2013/Accepted: 2 July 2014
ABSTRACT
Bio-pesticides are becoming
increasingly important as pest management tools in various cropping systems in
the tropics essentially to remedy problems associated with the indiscriminate
use of ‘hard’ and non-environmental friendly inorganic pesticide. In these past
few decades, many bio-pesticidal products, both microbial-based (bacteria,
fungi, microsprodia, entomopathogenic nematodes and viruses) and plant-based
botanicals (rotenone and azadiracthin) have been studied for their use against
insect pests in the tropics. In this study, the effects of the concentration
process with respect to the yield of rotenone (mg) and its concentration
(mg/mL) are presented extensively. The raw plants were collected from Kota
Johor Lama, Johor and sorted to obtain the roots and stems. Only the roots and
stems were utilized as raw materials of the extraction process. The rotenone
from roots and stems was extracted using the normal soaking extraction (NSE)
at 28 to 30oC with 95% (v/v) of acetone as
a solvent and the solvent-to-solid ratio of 10 mL/g. The extraction was carried
out for 24 h. Next, the liquid crude extract was concentrated using the rotary
evaporator at 50oC and 80 mbar of vacuum pressure to
remove approximately 90% of solvent. The fractions of the liquid crude extract
were collected (15 min/mL/fraction), diluted (1/100 with acetone) and cleaned
up (to remove any fine debris) prior to determination of rotenone content (mg)
and concentration (mg/mL) by using the reverse-phase high performance liquid
chromatography (RP-HPLC). Finally, the results showed
that there was a significant effect of thermal degradation or dissipation of
rotenone content at higher operating temperature (greater than 40oC)
with a rapid rotenone reduction for the first 15 min of exposure. The
possibilities for better exploitation and identification of the effective
operating parameters based on the above mentioned results will be perhaps
discussed in the future.
Keywords: Concentrated liquid crude
extract; Derris elliptica; rotenone; thermal degradation
ABSTRAK
Bio-pestisid pada masa ini sedang mengalami
peningkatan yang sangat penting sebagai kaedah mengawal makhluk
perosak dalam variasi sistem tanaman tropika terutamanya sebagai
jalan untuk mengatasi masalah yang berkaitan dengan penyalahgunaan
pestisid bahan bukan organik berat yang tidak mesra alam. Dalam
beberapa dekad yang lalu, banyak produk bio-pestisid, kedua-duanya
bagi basis mikrob (bakteria, kulat, mikrosprodia, entomopatogenik
nematod dan virus) dan bahan botani berasaskan tumbuhan (rotenon dan azadiraktin)
telah dikaji berkesan untuk kegunaan serangga perosak dalam iklim
tropika. Dalam kajian ini, kesan daripada proses pemekatan terhadap
keberhasilan rotenon (mg) dan kepekatannya (mg/mL) telah dikaji
secara menyeluruh. Sumber pokok mentah dikumpulkan dari Kota Johor
Lama, Johor dan diasingkan untuk pengumpulan akar dan batang. Hanya
akar dan batang sahaja digunakan sebagai sumber bahan mentah untuk
proses pengekstrakan. Rotenon daripada bahagian akar dan batang
diekstrak menggunakan pengekstrakan celuran norma pada suhu bilik
iaitu 28 to 30oC dengan 95% (v/v) aseton
sebagai pelarut dan nisbah pelarut-kepada-pepejal bagi proses pengekstrakkan
adalah 10 mL/g. Proses pengekstrakan dijalankan selama 1440 min.
Seterusnya, cecair ekstrak mentah dipekatkan menggunakan alat penyejatan
berpusing pada suhu 50oC dan tekanan vakum 80 mbar untuk mengeluarkan
pelarut aseton sebanyak lebih kurang 90%. Fraksi cecair ekstrak
mentah dikumpulkan (15 min/mL/fraksi), dicairkan (1/100 dengan aseton)
dan ditapis (untuk membuang sebarang habuk halus) sebelum proses
analisis kandungan rotenon (mg) dan kepekatannya (mg/mL) menggunakan
fasa terbalik cecair kromatografi berprestasi tinggi (HPLC). Akhirnya, keputusan uji
kaji menunjukkan bahawa terdapat kesan signifikan degradasi terma
terhadap kandungan rotenon pada suhu operasi tinggi (melebihi 40oC)
dengan kadar pengurangan pantas rotenon pada 15 min pertama operasi.
Kebarangkalian untuk mengkaji dan mengenal pasti parameter operasi
yang lebih effektif berdasarkan kepada keputusan uji kaji ini akan
dibincangkan kelak.
Kata
kunci: Cecair ekstrak mentah pekat; degradasi terma; Derris elliptica; rotenon
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*Corresponding author; email: saiful-z@ukm.edu.my
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