Indian Journal of Agricultural Sciences 80 (5): 405–8, May 2010

Field appraisal of controlled release formulations of cartap hydrochloride against

rice leaf folder (Cnaphalocrocis medinalis)
JITENDRA KUMAR1, NA SHAKIL2, SUBHASH CHANDER3, SURESH WALIA4,
LIVLEEN SHUKLA5 and BALRAJ S PARMAR6

Indian Agricultural Research Institute, New Delhi 110 012

Received: 25 November 2009; Accepted: 4 March 2010

ABSTRACT
An experiment was conducted during 2005 to study the bioefficacy of controlled release formulations of cartap
hydrochloride (2-dimethylaminopropane-1, 3-diol) against the rice leaf folder [Cnaphalocrocis medinalis (Guenee)].
Controlled release formulations of insecticide cartap hydrochloride were prepared using commercially available polyvinyl
chloride (emulsion and suspension), carboxy methyl cellulose and carboxy methyl cellulose with clay (bentonite, kaolinite
and Fullers’ earth). These released cartap hydrochloride beyond 45 days as compared to 14 days from its commercial
4G. sodium carboxy Methyl cellulose-Kaolinite-based formulation provided a superior control (3.33%) of rice leaf
folder in field grown rice (Oryza sativa L.) at half the dose (375 g a i/ha) in comparison to cartap hydrochloride 4 G
(5.44%) at 72 days after treatment. The residue of cartap hydrochloride was detected below maximum residue limit of
0.1 mg/kg in grain 72 days after its application.

Key words: Cartap hydrochloride, Controlled release formulation, Polymeric matrices, Rice, Rice leaf folder

Cartap hydrochloride (2-dimethylaminopropane-1, 3-diol) It is currently controlled by spraying the crop with
is a systemic insecticide for soil. To achieve control of insects, thiamethoxam, monocrotophos, aldicarb, carbofuran,
it is necessary to maintain regulated supply of an appropriate profenphos, lambda cyhalothrin, phorate etc. In view of the
concentration of chemical in the plant rhizosphere. To counter large area under rice crop in India, its pest problems and
environmental losses and maintain the concentration above insecticide consumption, the controlled release formulations
the minimum threshold of activity, application of excessive of cartap hydrochloride were developed and evaluated for
amount of conventional formulation of cartap hydrochloride its efficacy for the management of rice leaf folder along with
is required. Increase in application rate, however, results in its commercial formulation 4G (4% ai) in rice (Oryza sativa
an increase in the potential adverse impact on the L.) field during the rainy season of 2006 at Indian Agricultural
environment. Controlled release formulations can ameliorate Research Institute, New Delhi.
pesticide losses due to leaching, evaporation, degradation
MATERIALS AND METHODS
etc (Fernandez-Perez et al. 2000) and thus maintain toxicant
levels above the minimum threshold for long. Due to the Commercial grade bentonite, kaolinite and Fullers’ earth
various advantages, numerous examples are available in (MCA Industries, New Delhi, India), carboxy methyl
literature wherein such products have been effectively cellulose-Na (Merck India Ltd, Mumbai), polyvinyl chloride
employed to combat the pests (Mulqueen 1998, Kumar et emulsion and polyvinyl chloride suspension (Choudhary
al. 2003a). Field appraisal of controlled release formulation Polycoats, Bahadurgarh, Haryana) were used. Cartap
of phorate and carbofuran against the rice leaf folder hydrochloride (Technical Grade) with purity of 85% w/w
[Cnaphalocrocis medinalis (Guenee)]. is also reported and commercial granules (4% a i) were obtained from its
(Kumar et al. 2003). manufacturer M/S Northern Minerals Ltd, Gurgaon. For
Rice leaf folder [C. medinalis (Guence)] is an important routine laboratory work, laboratory grade, and for HPLC
pest of rice and causes severe damage (60–70%) to the crop. analysis, analytical grade, chemicals and solvents were
employed.
1,2,3 SeniorScientist, 4 Principal Scientist, Division of Polyvinyl chloride suspension (PVC-suspension) and
Agricultural Chemicals; 5 Senior Scientist, Division of polyvinyl chloride emulsion (PVC-emulsion) were prepared
Microbiology; 6Former Joint Director (Research) as follows:
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406 KUMAR ET AL. [Indian Journal of Agricultural Sciences 80 (5)

The polymer (9.529 g), and cartap hydrochloride (0.471 formulations were broadcast in standing crop 20 days after
g, 85% purity) were dissolved in dichloromethane. The transplanting. The release of cartap hydrochloride from PVC-
solution was thoroughly mixed with a metal spatula. The Suspension and PVC-emulsion was relatively slower
slurry so formed was dried in a Petri-dish to yield a hard therefore was not included for bioefficacy study. The
mass which after drying was ground in a laboratory Wiley mill controlled release formulations (CMC, CMC-Kaolinite,
and then sieved to obtain granule of size 30/60-mesh size. CMC-Bentonite and CMC-Fullers’earth) were evaluated at
A mixture (104.71 g) of sodium carboxy methyl cellulose, 10, 5 and 2.5 g/4 m2; equivalent 750, 375 and 187.5 g a i/ha,
clay and cartap hydrochloride technical (85% purity) was respectively and the commercial 4G at 10 g/4 m2; equivalent
prepared in the ratio of 50:50: 4.71 by weight to obtain 4% a 750 a i g/ha only. Per cent leaf folder damage, 27 days after
i products and was mixed well in a mixer grinder. Water treatment, was recorded by counting the number of damaged
(250.0 ml) was added to it for making dough. For overcoming leaves/hill, before and after treatment, from 10 randomly
stickiness, 51.0 ml of aluminium sulphate (0.5 M) was added selected hills in each plot. Observations were similarly
as a gelling agent. The resultant mass (120.82 g) was dried recorded at 27, 42, 57 and 72 days after treatment. The leaf
at 40°C in an oven. The dried mass was ground in a laboratory folder damage (%) was calculated as follows:
Wiley mill and sieved to obtain particle of 30/60-mesh size. Damaged leaves/10 hills
To Prepare sodium carboxy methyl cellulose-based Leaf-folder damage (%) = ×100
Total leaves/10 hills
formulations one mixture of sodium carboxy methyl cellulose
and cartap hydrochloride technical (85% purity) was prepared Cartap hydrochloride (25 mg) of analytical grade was
in the ratio of 100: 4.71 by weight to obtain 4% a i products weighed and dissolved in 50 ml of distilled water in a
and was mixed well in a mixer grinder. The mixture was volumetric flask to make 500 ppm solution. To this solution
processed as in sodium carboxy methyl cellulose clay-based 5 ml of nickelous chloride solution and 5 ml of concentrated
formulations. ammonium hydroxide were added and shaken for 30 min.
The content of cartap hydrochloride in developed products The nereistoxin was extracted twice with 25 ml of n-hexane
was estimated. Granules (250 mg) of CMC and CMC-clay- by the separating funnel, hexane was removed and residue
based formulations were treated with acetonitrile (15 ml) in was dissolved in acetonitrile. Convergence of cartap
an ultrasound bath for 10 min. This led to the complete hydrochloride into nereistoxin was confirmed based on their
disintegration of the granules. After an interval of 2 hr at respective retention time 3.86 min. and 4.26 min. by HPLC
room temperature, the mixture was sonicated again for 10 analysis (Shimadzu). The nereistoxin thus formed was used
min (2 times) and was then filtered quantitatively through a as standard.
syringe filter (0.2 μm). The volume was made up to 10.0 ml. The straw and grain samples at harvest were air-dried at
A 250 mg sample of PVC-Suspension and PVC –Emulsion room temperature and stored at –20°C before analysis. The
was refluxed for 6 h in acetone and filtered. Acetone was cartap hydrochloride residues in straw and grain were
removed from the filtrate at 30°C in a rotavapor under estimated separately. A representative chopped sample
reduced pressure. The residue was taken in acetonitrile and (25 g) of straw/ground rice grain (25 g) was homogenized
was then filtered quantitatively through a syringe filter (0.2 with 200 ml (0.02 M HCl) in a mixer grinder for 15 min.
μm). Recovery of cartap hydrochloride from different CR at a high speed. It was filtered through Bückner funnel
formulations varied from 90.4 to 98.6%. under suction. The residue was taken back in mixer grinder
Cartap hydrochloride was estimated using a Shimadzu and extraction repeated with a fresh lot of 200 ml (0.02 M
high performance liquid chromatograph (HPLC) fitted with HCl). Each mixture was shaken with 5 ml of 2% nickel
SPDM6A Photodiode array detector. Samples were resolved chloride solution and 5 ml of concentrated ammonium
isocratically on a 15 cm × 3.9 mm id RP 18 column using hydroxide for 15 min. The extracts were combined and the
acetonitrile-water (70:30) at 1 ml/min as mobile phase. The aqueous phase was extracted twice with 100 ml n-hexane.
absorbance was recorded at 276 nm at sensitivity of 0.05 The aqueous layer (lower) was discarded. The organic layer
AUFS by injecting a volume of 20 μl. (upper) was filtered dried by passing through 2 cm layer of
It was studied as per Fernandez-Perez et al. (2000) and anhydrous sodium sulphate, concentrated and subjected to
Choudhary et al. (2006). For comparison, the term ai release GLC analysis.
was considered as the amount of active ingredient recorded
RESULTS AND DISCUSSION
at a given time. The release was studied in comparison with
the commercial granular formulation. Release of cartap hydrochloride in soil
The nursery of ‘Pusa Sugandh 3’ rice susceptible to rice Periodic release of cartap hydrochloride from the test
leaf folder was raised and transplanted during the rainy season polymeric products along with its commercial formulation
of 2005 following a simple randomized block design with 3 4G in soil is presented in Fig 1. The rate of release from
replicates. The plot size was 2 m × 2 m. The rows and plants controlled release formulations were much slower than
were spaced 20 and 15 cm apart, respectively. All the commercial formulation 4G, which achieved its maximum
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 May 2010]BIOEFFICACY OF CONTROLLED RELEASE FORMULATIONS OF CARTAP HYDROCHLORIDE AGAINST RICE 407

CMC CMC+Kaolinite CMC+Bentonite available beyond 42 days. Carboxy methyl cellulose released
CMC+Fullers'earth Comm.4G PVC-Suspension cartap hydrochloride faster than the other polymers, polyvinyl
PVC-Emulsion chloride emulsion and polyvinyl chloride suspension being
100.0 the slowest. Linear release was evident during the first 30
days (CMC and CMC-clay), and 42 days in other polymers.
80.0 After this, the rate decreased sharply in carboxy methyl
Cumulative release (%)

cellulose and other carboxy methyl cellulose-clay-based

60.0 formulations. It appears that on complete release of cartap
hydrochloride from the controlled release formulations, its
40.0
degradation occurred fast in soil (30–42 days) in
20.0 carboxymethyl cellulose formulations. Carboxy methyl
cellulose showing faster release is hydrophilic in nature and
0.0 is easily biodegradable (Cotterill et al. 1996). The
10 20 30 40 50 hydrophobic polymers with cross-linked matrices such as
–20.0 Days PVC emulsion and PVC suspension showed slower release.
Fig 1 Rate of release of cartap hydrochloride in soil from controlled Similar results have been reported with diuron granules based
release and commercial formulations on lignin (Cotterill et al. 1996), phorate on polyvinyl,
polystyrene, cellulose acetate and polyethylene glycol 6000
release of active ingredient by day 12 and 18 in water and (Rao 1992) and butachlor on ethyl cellulose and polyvinyl
soil, respectively after which the ai content decreased, matrices (Kumar et al. 2003a). All CMC-clay formulations
probably because of its degradation. In contrast cartap showed slower release in comparison to CMC alone up to
hydrochloride content increased gradually in all the 28 days. It is evident that the incorporation of clay in CMC
polymeric formulations. The release followed the order: slowdowns the release of cartap hydrochloride.
Commercial formulation 4G > CMC > CMC-Kaolinite >
CMC-Bentonite > CMC-Fullers’earth > PVC emulsion> Field evaluation
PVC suspension. All the treatments gave a significantly superior control of
It is apparent that so long as cartap hydrochloride is the pest over the untreated control at 27, 42, 57 and 72 days
retained in a stable polymeric structure, it is protected from after transplanting (Table 1). The CMC-Kaolinite @ 10 g
various biotic and abiotic losses. In case of commercial (T 5 ) was significantly superior to all the treatments
formulation 4G, the cartap hydrochloride was detectable up throughout the observations. The treatments cartap
to 30 days, whereas in the polymeric formulations, it was hydrochloride 4G (@ 10 g (T1), CMC @ 10 g (T2) and CMC-

Table 1 Bioefficacy of controlled release and commercial cartap hydrochloride 4G formulations against rice folder [Cnaphalocrocis medinalis
(Guenee)]

Treatment Pre-treatment Folded leaves/10 hills (%)

count
27DAT 42DAT 57 DAT 72DAT

Control a3.89 (0.47) a16.89 (8.46) a23.17(15.50) a 25.55(18.62) a26.21(19.52)

T1 Cartap hydrochloride 4G (10g) a3.37(0.27) fg2.99 (0.27) f6.16 (1.15) fgh10.52 (3.34) def13.47 (5.44)
T2 CMC(10g) a 2.49(0.22) fg 3.15 (0.31) cd7.75(1.82) fgh 10.30 (3.20) def 13.39 (5.38)
T3 CMC(5g) a 2.99 (0.24) ef 3.89 (0.47) c8.92 (2.41) d12.19 (4.47) c15.30(6.97)

T4 CMC(2.5 g) a 3.04 (0.28) d e4.31(0.57) b11.03 (3.67) b15.12 (6.82) b18.82(10.42)

T5 CMC-Kaolinite (10g) a 2.92 (0.26) g2.21 (0.15) g5.06 (0.78) i8.88 (2.39) h10.51(3.33)

T6 CMC-Kaolinite (5g) a3.74(0.447) ef4.11(0.51) f6.29 (1.20) gh 10.13 (3.10) fg12.22(4.49)

T7 CMC-Kaolinite (2.5g) a 3.13 (0.33) d5.28(0.85) cde7.99 (1.94) ef11.14 (3.74) cde14.13(5.96)

T8 CMC-Bentonite (10g) a 2.95 (0.31) fg3.10(0.29) ef6.96(1.47) hi9.68 (2.83) gh11.10 (3.71)

T9 CMC-Bentonite (5.0g) a 3.54(0.38) d e4.70(0.67) cd8.54(2.21) fgh10.29 (3.19) ef13.15(5.19)

T10 CMC-Bentonite (2.5g) a 3.57 (0.41) c6.69(1.36) b10.52 (3.35) cd11.94 (4.29) cd14.59 (6.35)

T11 CMC-Fullers’earth (10g) a 3.02 (0.30) d e4.76(0.69) de7.65(1.77) fg 10.01 (3.03) f12.61 (4.77)

T12 CMC-Fullers’earth (5.0g) a 3.35(0.35) c6.75(1.38) cd8.65(2.26) fg10.68(3.44) cd14.628(6.39)

T13 CMC-Fullers’earth (2.5g) a 3.69(0.42) b7.97(1.93) b10.77(3.50) c13.49 (5.45) b17.41 (8.97)

Tukey’s HSD 2.62 1.11 1.07 0.94 1.41

Prob.>F(trt) 0.83 <.0001 <.0001 <.0001 <.0001

DAT, Days after transplanting; Values in parentheses are mean values

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408 KUMAR ET AL. [Indian Journal of Agricultural Sciences 80 (5)

Bentonite @ 10 g (T8) were statistically at par at 27 days Table 2 Cartap hydrochloride residues in rice straw and seed after
after transplanting and were most effective than other harvesting
treatments except T5 which was the best. At 42 days after
Treatment Average residues (mg/kg)
transplanting, cartap hydrochloride 4G (@ 10 g (T1) and
CMC-Kaolinite @ 5 g (T6) were at par, followed by CMC- Straw Grain
Bentonite @ 10 g (T 8). The treatments CMC @ 2.5 g Control 0.00 0.00
(T4), CMC-Bentonite @ 2.5 g (T10) and CMC-Fullers’ T1; Cartap hydrochloride 4G (10 g) 0.051 0.031
earth @ 2.5 g (T13) were least effective but significantly T2; CMC (10 g) 0.032 0.020
superior to control. The treatments CMC-Kaolinite @ 5 g T3; CMC (5 g) 0.012 ND
(T 6 ) and CMC-Bentonite @ 10 g (T 8 ) provided a T4; CMC (2.5 g) ND ND
T5; CMC-Kaolinite (10 g) 0.027 0.018
superior control than cartap hydrochloride 4G (@ 10 g (T1) T6; CMC-Kaolinite (5 g) 0.011 ND
at 52 days after transplanting whereas CMC @ 10 g (T2), T7; CMC-Kaolinite (2.5 g) ND ND
CMC-Bentonite @ 5 g (T9), CMC-Fullers’earth @ 10 g (T11) T8; CMC-Bentonite (10 g) 0.024 0.015
and CMC-Fullers’earth @ 5 g (T12) were at par. At 72 T9; CMC-Bentonite (5.0 g) 0.010 ND
days after transplanting, T5 followed by T6 and T11 were T10; CMC-Bentonite (2.5 g) ND ND
T11; CMC-Fullers’ earth (10 g) 0.020 0.011
the best treatments. The treatments T 1, T 2, T 7 and T 9 T12; CMC-Fullers’ earth (5.0 g) ND ND
were statistically at par and better than other treatments T13; CMC-Fullers’ earth (2.5 g) ND ND
(T3, T4 and T13). The CMC-Kaolinite @ 2.5 g (T7) also
provided at par control than cartap hydrochloride 4G (@ 10 ND, Not detectable; CMC, sodium carboxy methyl cellulose
g (T1).
and load in the environment.
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