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Cl~npter 3 DETERMINATION OF PROPOXUR

Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

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Page 1: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

Cl~npter 3

DETERMINATION OF PROPOXUR

Page 2: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

l'roposur, 2-(1-111c1l1ylctl1osy) plic~iyl ti~ciliyl carbaoi:~te ( I 14-26-1) belongs to

cnrbnn~i~tr: class i~fpcstici(les.

I'ropoxur was synthcsizcd by Rockcr (1) by the reaction of u-isoprol~oxy plienol with

Prol)oxur wns dcvcloped as n Cl~cmt~gro's parent by Leverknsen. It was

i~ltrorluced in market by Bayer, AG as code No, "Bayer 09007","5812315". Propoxur is

know1 by thc common name 'Arprocab' and the tmde nomes 'Raygon' i~nd LBlaLlane~'

ill house llold and public health; 'Unden' and 'Undenc' in agriculture.

Propoxur is u wliile or cmam coloured crystnlli~~e solid with a 111ild pllel~olic

odour (Tcclinical); n1.p. 91°C, sparil~gly soluble in water (2 giL at 2 5 ' ~ ) and readily

solublc ill lllost of' t l ~ c organic solvents. Prol~oxur is co~~~mcrc ia l ly avaiiablc as 1%

Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~ert ies o f

propoxur were studied by Unterstenhofer (2). It Is a non-systemic insecticide with rapid

knock down. It is liiglily cffcctive against ai~ts, api~ids, bugs, cockroaclies, flies, jassids,

multipcd, rnosquitocs and otllcr household public health pests, ectoparasites on dogs and

poultry. It is highly toxic to honey becs. Propoxur's mute Loxicily is low for marnluals

(3). Acute LDro for rat is 800-1000 tnglkg. Bioactivity and persistence of propoxur in

lllincrnl soil, riverbeds atid in tllc i~qut~tic c ~ i v i r o ~ ~ ~ i i o n t linvc been sulnmarizcd (4-6).

Baygon applied to soil has sliowl~ systclnic actioli against t l~rips aphids, leaf miners, leaf

hoppers and scales (7).

Page 3: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

.1.llc rzic~ tll;~t lllc cxccss lee of c;;~biimnlc pcsliciilcs icods to cnvirolnlnclltal

pol~u~;ull . 1, neccssil;l[cs d c v o l o p ~ ~ ~ c ~ ~ t of liovel ~~ lc t l~ods lor tllc dctarnifl;iiioil Llle

ing~rdicnrs i r ~ ~ n r ~ u l ; ~ ~ i o o , s to assess the qodity, quantity slid colltrol of these

pcsticiiies.

Scveral mctl~r>ds l~avc bccn icportcd for the idc~~tif icat io~~ and qua~llitativc

dctcnnination of propoxur. Miskus ct nl., (8) rcported a colorimetric and papcr

cii~.o~~iatograpliic mctllod Tor tlie dctelmination or cnrbamates usil~g 4-ni~ohenzene

diazoniun~fluoroirorane. Sut,uki ct al., (9) pccser~led n scheme Car the s~steoiatic

idenlilication of 13 c~~sl'i~iaate rcsidl~cs I I I I ~ ibeir d c t ~ l . ~ ~ ~ i ~ ~ n t i o ~ ~ . Pe~.et;? (10) tlcscl ibcd a

calurimctric techllique for propoxur utilizing 3-nitroanilinc 4-sulphonic acid as a

colouring ugcnt. Kcit11 and Alford (I 1) l~ave cataloged higii resolutio~l NMR spectra of

35 carbamcltc pesticides and their mclabalites. Val1 Gils (12) rleveloped a

spectrop1~otometric procodurc for thc detcnnination of propoxur residues on vegetable

mutter. El - Dib (13) described u TLC lecliniquc for thc assay of c:lrbamatc and phenyl

urea peslicide residues in onturn1 willers, An AC poliuogniphic tecl~nique for the

determination of ~iietliyl carbnmnte pesticides including propoxur was reported by Booth

and Fleet (14). Gwiaztla (15) detennined propoxur by developil~g 1R spectrophotometric

mcthod. Lawrelice and Frei (16) described TLC teclinique for the determination of

carbarnates as floiuoscent I-dimethyianii~~o~iaplitl~ale~ic 5-sulphonate esters. Stanley et

al., (17) h v c successfuily utilized gas cl~rnrnatograpi~y for the determination of propoxur

residues and its ~iietabolites in plant tissues. Stanley and Tl~or~lton (18) dctermilled

propoxur residues ar~d ilu rnctabolitcs ill anin~al tissues nnd milk by clcctron capture

detection by GC. A GLC method or tho analysis of carbanlate pesticides and phenolic

conlpolulds in water was reported by Blagg and Rawis (19). Ueje atid Knnazawa (20)

~lalyzed trifluoro derivatives of propoxur and its metabolites by ECD. Viekcn et al.,

(21) havo studied the laser excited Ruman and fluorescence spectra of propoxur and other

pesticides, lshi and Otake (22) elnployd !IPL,C teclnique for the analysis of pmpoxur.

GC metllod with electron capture cictcctor WIIS utiiizcd by I-Ioldei~ (23) for the

determination of 2,4.dinit1~opl~enylet11er derivative of propox~u ru~d its metabolites.

Runaswnmy (24) described a colorirnefric niethod to determine eight cabalnates

including ProPoXur, 4arnino 3-nitrobenzenesull,bonic acid was the couplillg agent,

Page 4: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

llolden (25) rcjlc~rtcd ;I OC ~nctliod for t l ~ c deternii~~ation oE2,4-dinitropl1e11yl ether lllulti

resid~~e of propoxur wit11 olllcr ca~b;~ti~ate 1)esticides in crops. S~~lpholiic acid was

employcrl ns it co lo i~r i~~g azo dye rcagcnt for the colori~lletric deter~~iinat io~i of propoxur.

Mokl~ct:jec et ill., (26). Ems1 el ai., (27) described n TLC enzyme inhibition technique for

tllo aoi~lysis of pro1)oxur. I'iccl~oka (28) developed ti colorimetric method to dc te~mi~ic the

propoxur in potatoes usic~g 4-amino antipyrine ns 11 uzocoupling agent. Joshi and Jogickar

(29) tlctor~ninctl the carbaryl and propoxur by eoloriinetric nlcthod. Kubocki ct al., (30)

used GC wit11 EC dctcetor to csti~ilate prapoxnr and carbofura~~ residues in vegetables,

raw niaierinls and byproducts.

Cobur~l et al., (31) outtilled a GLC with ECU tilethod to rleler~iii~ie N-methyl

carbarnate pesticides in natural waters. Moye et al., (32) dcsigned a dynutnic fluorogenic

iabeling detector for III'LC analysis of six N-mcthyl carbatnates and two cnrbaryl oxide

pesticitles. Schoene and Steitdlanses (33) rcpartcd n s j i c c t r o ~ ~ l ~ o t o ~ ~ ~ e t r i c method for the

quantilativc analysis o r N-mono substituietl carbarnrites including prapoxur. Miyumolo

et a!., (34) osed n inulti rcsidoe a~ialyticnl incthorl for the detel.tninatiolt of N-methyl

cnrba~liate pesticides. Kikta and tlebst (35) tiescribed an internal slalltlartl I-IPLC method

for the determination of propoxur. ficclmiak and Foss (36) designed GC method to

dctermi~~c propoxur and iso-propoxy phenol in blood, urine and tissues. GC with flame

themiionic detector for the dctcrtni~~ation of carbatnate pesticide residues in food material

was described by Yoshida ct al., (37). Fogy el al., (38) described a multi dimcnsionsi

I-IPLC method for tlle deterlnlnntion of carbarnate i~isecticides in fruits and vegetables.

Vw dor lloli nnd Lnge~nnnt (39) reported n ctirccl d c t c r ~ ~ ~ i ~ i u l i o ~ i of propoxur ill p l ~ ~ n t

tissues by GC [nethod with an alkali FID, A sensitive method Cor the analysis of eight

oarbaniale iriseclicide residues in foliage, forest soil and fish tissues by direct GLC with

N1-PD was developed by Szeto and Sundaralii (40). A general TLC melhod is tlcveloped

by Ambrus ct al., (41) to deternine the carbaniate pesticide residues of plant origin, air

and water samples. ficixa and Marti (42) developed a coloritnetric procedure for tile

analysis of carbnryl, propoxor, cflllto~i and Ca(CN)z in air. Appaiah et al., (43) followed

coloritnetric procedure for the determination of prapoxur aud its residues in vegetables

uslng 4,4-dinminodipl1enylsulpi1otie ns a coupiiiig agent, with good sensitivity. Tratltweil~

and Guyon (44) developed a simple, direct and sel~sitive at low te~i~perature

Page 5: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

l ~ ~ ~ o s ~ ~ l ~ o r i m e t r i c inctl~od io tlctcrminc propoxur. l l i l l ct. nl., (45) cmploycd liquid

chrornningln]~hy technique wit11 post coIun111 iluorcscc~~cc dcrivatioll fol the

dctennination of N-metl~yl c:lrb:~!,,:~tc p~~~;ticirli~,: i i , !,!ell w.v;ll,,-. A tIie~~~ir~!:l)~.ilv OC-MS

spectra of 15 carhamatcs'~wos s ~ , , i ~ r i l ;an<l ~ I I , , r l i t i i \v,ls ii,,~:ci 1 0 1 I I L C d ~ . l t ~ ~ l i l i i l , i l ~ ~ > ~ ~ of the

pcsticides by Voyksner et al., (46). Kr:~usc (47) rlcvclopccl a incilic~el for tllc rlctcl~~ninatioil

of carbi~mates in crops. Appaii~h ct ul., (48) described a colo~~imclric method for the

detcrnii~~ntion of propoxur resirlues in vegeiablcs and watel..

A rnpid capillary super critical fluid chmn~atographic luctl~od of analysis of

crrbamute pesticides wils dcscribetl by Wright and Smith (49). I1ropoxur i~isccticidc

was ru~alyzed by Lesser el a]., (SO). The technique involving tlic saponification of the

cnrban~ate insecticide with 0.01M NaOH at 8 0 ' ~ and then mixing with phthalaldehyde

reagent in preseiice of a ~iiercaptoetl~anol was reported by Engelliardt ru~d Lilling (51).

Stamp et al., (52) obtained inass spectra of 20 carba~nates pesticides using chcmical

ionization tecluiique. Sastry et al., (53) developed a sensitive spectrophotometric

technique for tlie determination of carbaryl and propoxur in formulations, water and

grains using p-dimnethylaminobenznldel~yde and p-dirnethylamino cinnamaldel~yde. A

spectrophotometric method was developed by Sastry and Vijaya (54) to determine the

propoxur, carbaryl, fenithrothion and niethyl parathion with 3-methyl-2-benzothimlino-

hydrazone hydrochloride. The same authors (55) have also reliorted a speclropl~otometric

~nethod for tlie determiiiation of propoxur r~nd carbaryl using a ~ ~ i i ~ l o p h e ~ i o l anel phenylene

tliamioe, Goewie and Hogeildoor~i (56) developed an automated I-IPLC method to

determi~ie tllc propuxur and oll~cr carbamatcs in total diet sample cxtrect. A dircct GC

method for the detcrminatio~i of carba~nate pesticides and its for~nulalions was ~.eported

by Sukune (57). Branckhoff aud Their (58) described GC inell~od to deteunirie IS N-

metl~yl carbnmates and four metabolitcs in fillits and vegetables. Wachhole et al., (59)

described HPLC-PTIR olilinc coul)ling 111clhod for the a~ialysis of cmbalnate insecticides,

A si~nplified mulli residuc liquid chro~natograpl~ic neth hod for the determination o f seven

N-methyl cnrbamntcs t~long wit11 propoxur In vcgctal~les a~itl Guits was tlcvelopcd by

Daniel Chaput (60). Naidu and Naidu (61) used spectiopl~otometric method for the

dcteh~iii~atian of cnrbosulfru~ ood propoxur using 2-mlino benzophenone as a c o u p l i ~ ~ g

%agent. Raju mid ALmham (62) developed a rapid and scnsilive spectrophotometric

Page 6: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

et nl., (63) adopted flow injection spcctrol>boto~~~ctric tcchniqoc lo determine tile

propoxur and its ~nctabolites withp-aminopl~enol. l'he same autlio~s (64) l ~ i ~ v e discussccl

the inleraction of propoxur and its ~nelabolitcs with surfactants. Agrawal anti Gupla (65)

described n higl~ly scicctive and rapid spcctro~>l~oto~nctric mcll~od Tor lllc tlctc!.minalion

of 11ro~~oxt". ill vegetables and graims. 'The partial least-sqnare calibrt~liot~ method for

siinulla~~cous killclic l l c ~ c s t i ~ i ~ ~ n t i o ~ ~ of projloxur, c;nb;~ryl, c~hio-l j~lct~rb and l i~ r~nc ln~~ulc

wi~s i~pplied by Garcia et al., (66). Dclago;~rdia, M.ct nl., (67) rlevelopcrl :I clc;in analytical

(68-69) reporled llle sensitive ~~eclrophoto~neiric ~lietllod for the detemiination of

propoxur using 4-mninu ontipyrctrc os n coupling rcagcnt. 1h1ju ct sl., (70) rcportcd a

rapid and sc~isilivc scrcc~ling mclhod lo dclcr~oiiic llic carbaryl nntl 11ropox~11. l~siirg 11-

~~itroaniline as a coupling agcnt. Hari Krishoa and Naidu (71) developed a simple

spectrophotomelric mcthod for the deler~~~i~linalion orpropoxur in water arid grains using

paracl~loronnilinc as n coupling agctil. Pmbhaknr Roo et al., (72) rcportcd simplc and

se~isilive speclropl~otometric deln?nination of cnrbomnle pesticides includi~lg j>~oposu~. in

its formulation and various vegetable samples with 2,4,6 - tribromo plicnyl hydrnzene us

a coupling agent. I-lnmscl~cr ct al., (73) prcsel~tcd n scnsitivc and selcctivc liquid

chromatograpl~ic mcthod ibr the detection of propoxur residues in eggs. I-Iari I(ris11na and

co-workers (74) reportcd a spectropl~oto~~~etric tcchniq~ic for monitoring of propoxur and

corbosulfnn in water sanples. Hcmasmidar atid Naidu (75) devclopcd a sensitive

spectrophotometric method for the determination of propoxur in its fornlulation and

water snn~plcs will] 3-ornit~opyridine.

3.2. Mntcrinls anti Methods

All chemicals used were of analyticnl grade. I'ropoxur was supplied by Bayer

India Limited, India. Preparation of stock and working reagellt solutions were shown in

Cllapler I1 io Section 2.1 and oppctldix I & 11.

Transfer 0.25 - 2.5 ml portions of standard prolioxur (10 pg ml") solution into a

series of 25 ml calibrated flasks. 2.5 ml of 2% NaOLI solution was added and allowed to

stand for complete hydrolysis of propoxur. The pI-I of the test solution was adjusted to 9.5

by adding 2.5 ml of phosphate buffer solulion and requisite amount of HCI followed Ly

Page 7: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

o~lrmol~ia solution. 2 ml of 0.2 % 4-n~etl~oxyaniline solution and 1.5 1111 of 10%

KIIPe(CN)s] were added and n~ixcd well to devclop colnureci co~n~~ounds . 'nie

absorbance of tllc colourcd proilucl was moasurcd s~~ectrophoio~ncirica~lly a( 425 nm

agoinst reagent blank. Si~liilar pracedi~re was adapted io rcni i~i~~ing cuupling reagenls

employed for these studies. The commercial forninlations of propoxur (1% oil based

spray, 2% bait nnd 20% wellublc powdel; forrificcl sn~nples of wnter, gl.ains and peas

were determined s~ctropl!oto~net~ically followi:~g tile procalure sl~own in Chaplur I1 in

Scction 2.9,2.1 1-2.12.

3.3. Rcsults

The optical nlhuacteristics of spectropliotomoiric measuremc~~ts of the coloured

producis formcd, on tllc alkali hydrolysis of propoxur N I ~ coupli~lg tile rcuulling

phenolic c o ~ n p o u ~ ~ d wit11 4-1iiclhoxynnili11e, 2,li-~Ii1ncthunp11~ili110, 4-nmi11obcn~ald~:I1ydc

and 2,6-dibromo-4-111ethoxyaniIinc in prcscacc of K][Fc(CN)h] at pl-I 9.5, arc

incorporated in tables 3.1 - 3.4. Delerminatio~~ of propoxur active ingredient io

insecticidal comme~cial fo~.~nulations, fortificti samplcs of water, grains and vegetable by

the method proposed are presei~ted in tables 3.5 - 3.16, The statistical importance of

precision and accuracy of tlie methods were ascettaincd by Stucient'~ 1 and F-iests and

data is presented in table 3.17.

Page 8: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

Table - 3 .I

Determination of Propoxur by oxidative coul~ling with 4.1nethoxyatiilinc

1.

2

3

4

5

6

7

8

Concentration range (ppni)

h ma* (om)

Colour stubilily (hrs.)

Molar i~bsorptivily ( L / mole, cm)

Sandell's sensitivity (pg/cm')

Relalive stnndard deviation (10 samples)

Correlation coeCficielit

% Rclativc error

0.4 - 11

467

48 --

2 . 9 9 ~ 1 0 ~

0.294 -

1.22

1 ,0000

1.03

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Table - 3.2

Detwminnlion of psopoxur. by oxidalive coupling will] 2,4-tlirt1cllioxy;111iii11c

Colour stability (Ills.)

Conce~itration range (ppo~)

1

4 Molar absorptivity ( L I nlolc, an) I 2.990~10 '

0.1- 12

Sandell's se~lsilivity (lrglcm2)

Relative stmldard dcv~atiorl (I0 samples)

Carrelalion coelficient -

% Relntive error

0.0346

0.33 --

0.9993

0.26

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Tablc - 3.3

Deternii~iatioli ol'propoxur by oxidative coupling with 4-ami~iobalzt~ltleIiydc

I I , ConcenWatinn mnge (ppm)

h ,,,, (11111)

Colour stability (firs.)

1 I 1 Molar absorptivity ( L i mole, cni)

1 6 I Itdative standard deviation (I0 samples) I

% Relative crror

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Ueter~ninotion of propoxur by oxidative col~pli~lg with 2,6-dibro~no - 4-metl~oxyaniline

1 1 C o l w stability (hrs,)

1.

% Relative error 1.35

Concentration range (ppm)

4

5

6

0.4 - 10.0

Molnr absorptivity ( L / male, cni)

Sandell's sensitivity (pdcn12)

Relative stalldud deviation (10 samples)

3.018~10'

0.0138

1.75

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Table -3.5

Determination af propoxur - Insecticide fomuhtions by uxiilalive coupling wit11 4-metlioxyani!jne

Sample Number

-

I .

2.

Lubeled amount

I"/. Daygon spmy

0.94

0.94

2% Daygo11 boil -- 1 3 2

1.92

20% Wellable !)(I W ~ C I '

19.84

19.84

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Table - 3.6 Dete~mination of propoxur - Ilrsecticidc for~liulolin~~s by oxitl:~livc col~l>li~lg will1 2,4.

dimetlioxyw~ilinc

Sainple Number

1 .

Labeled a ~ l ~ o u ~ l t

I % Baygon spray

0.93

2% B:lygon bait

1.85

20% Wct(iible powder

19.79

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Deiemiination of propoxur - I~isecticide fo~~mulations by oxidative coupling with 4 ainir~obcr~zoldel~yilc

Labeled amourit Sample Nulnber

1% Baygon spray 2% Raygo11 bait 20% WcUablc

1>0w<1er

1.84 19.62

0.96 1.85 19.66

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'l';ibic - 3.8 Detetniil~ation of propoxor - Insecticide fon~i~olntians by oxidative coupling wit11

2,6-dibronlo - 4-methoxynnili~~t:

Sample Number Lnbcled ornomlt I

20% Welti~blc 2% Baygon bait powdcr

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Table - 3.9

K E C O V C ~ ~ of propoxur from roriilied water s r ~ ~ ~ ~ p l c s using oxidative couplilig with 4-nieihaxyaoiline

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Recovery of propoxur from fortified water ssan~ples usi~lg oxidalive coupling with 2,4- dimelhaxyaniliiic

Stunple

Nutnber

1

2

3

L:orliiication

Level @pm)

0.4

0.8

1.2

Water samples

Tep wnler Distilled wntcr

Recovery

Amoimt (ppm)

0.38

0.71

1.09

5%

95.00

92.50

90.83

Amount (ppm)

0.36

0.73

1.08

%

90.00

9 1.25

90.00

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Recovery of propoxur from fortified water sal~iplcs using ux i~ l t~ t iv~ . coupli~lg wit11 4 nmi~~obcnzaldeliydc

Sample

Number

I I Water samplos --

I Distilled water

Level (ppm) Recovery

%

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Recovery of propuxur fio~il forlified water salupics osing axiill~tive coupling will1 2,G dibrolno 4-melhoxyaniline

I Water samplcs I

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Recovery of proljoxur corn grninv and vcgetnblcs using oxidnlive coupliug with 4-mothoxynniline

Rice Whcut I'cns Portificnliol~ -- -- - - -

Lcvcl Rccovcry

-

I -

Amount %

Ao~ount %

A111ount % (~~111) ( P P I ~ ) (PPI~) --

0.8 0.77 0.78 97.50 0.77 96.25

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Table- 3.14

Recovery of propoxur fro111 grains and vegetables using oxidative cuupling will1 2,4- di~nell~oxyaniiinc

I'cils Samplc Fortification - .~

Nu~~ibcr Lcvel 1tecovcry

Alnount Amount Amount

0.36

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Table- 3.15

Recove~y of propoxur from grains alid vegetables using oxidative coupling with 4- a~nininobenzaldel~yde

CiminsNegclnbles

Sn~iiple Poililicalio~~ Number Level

Recovery

I

2

.

0.6

1.2

%

95.00

95.67

Amoulit (PP~I )

0.57

1.15

%

95.00

95.83

Amount ( P P I )

0.58

1.16

%

96.67

96.67

Amount (~p1~)-

0.57

1.16

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Table- 3.16

Recovery of propoxur from grains and vegetables iisiiig oxidative coupling wit11 2,h- dibromo-4-methoxyanili~~e

Smnple Number

I

Fortificatiol~ Level

-- 0.5

Ricc

Recovery

Whcal

% _ I P P I ~ ) -

96.00

I'cns

Amount @pm)

0.46

-

%

92.00

Arnount

0.48

Amount ( P P ~ )

0.47

-

%

94.00

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Page 25: Cl~npter 3 DETERMINATION OF PROPOXURshodhganga.inflibnet.ac.in/bitstream/10603/39077/11/11...Daygon spray, 2% bnit, 4% Baygon and 20% wettable powder. Ilisecticidal p~ol~erties of

The absorption characterstics of the coloured products fornicd by tile pllc~~olic

product obtained on alkaline hydrolysis of propoxur with 4-a1etl1oxyanilinc, 2,1-

di~nethoxyol~iline, 4-minobenmldehyde and 2,6-dib1~1no-4-methoxyaoili1ie reveal that

these reagents can be successfully enlployed as coupli~lg agents, in the prescncc of

oxidizing agent Kd%(CN)6 for the determination of propoxur. These reagents find scvcrnl

advantages over the existing reagellts reported in tile literature. The greater stability of the

coloured compounds, free from interference, no need of solvcnts for the cxlr;~otio~~ of

coloured compo~uids, independent of temperature and less rengel~l consumption src sulnc

of the ~dvantages or Lhese reagents The molar absorptivity ol' the coloured cy;oiogcn

co~npounds fonlled ranges fro111 2.16 x 10' to 3.02 x 10' L mol"cm" indicating tlic

higl~er sensitivity of the n~etliods. Beer's law was obeyed ovcr the concentmtion range

0.3 - 12.0 ppm. The foreign species do not interfere with present ~nctllotls duc lo low

Sandell's sensitivity. Correlation eo-efficie~its we very close to unity. l'llis shows that

tile absorbance depends on Llle concentn~lion of the inseclici(le. Tile atldilio~l;il

advaitage oi'tl~e methods includes the instn~ltnneous fornlatioi~ of tlic colou~~ctl cyilnogcn

co~npounds at room tcmpcrature. The coionr remains stable for loager periods and offers

a better recovery tiIan those repo~ted by Vdllltateswarulu aiid Seshaial~ (68). The relative

standud deviation and percentage error velues are indicative of better precisinn and

i~ccuracy,

Based on the results pertaining to the reagents the spcctropliotomctric ~~ictliod is

extended to nlonitor tlie active ingredient in the available comme~cial foouulation or

propoxor. Furlhc~~, tlic observations suggcsl ll~ut tlic olhw ingrcdie~~ls pmselll in l l~c

formnlntion do not interfere, I~Ience, the selected reagents can bc successfully adopted for

a routine check up of the purity of the commercial insecticidal formulations.

The percentage recovery from the fortified water stuuples and grains ranges from

95,80% to 99.85 %, lrligll pcrcc~iklg&e rcveals thnl Lllc proposed ~iicthods are simple, riq~iil,

sensitive and inexpe~isive. Tl~c rccovp!.ic$ nsp fnl~onrably colnparerl with the rcporled

method (68). Further, the developed procedures do not itivolve elaborate clean LIP as

required by other methods (68 & 72).

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Tlie performances of t l ~ c proposed ~nethotls were moiiitored stntisticnlly io tcrms

of Student's t and F-tests of P values with the rel~mted rnotl~od (68). I t ~.evcals t l ~ n f the

proposed methods have no significant difference with reported method.

The proposed methods described here would serve as an addilion;~l tcchniquc for

the determination of propoxur in fortified samples of water, grains and vcgctables.

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