免费文献传递   相关文献

Study of deltamethrin detection method and its residual dynamics in Loincerae Japonicae Flos

溴氰菊酯残留测定方法及其在金银花中残留动态研究



全 文 :2016
y

z Ó
41
âÓ

}
Vol41,No.8 April,2016

st)(
] 20151110

†‡ˆR
] 


‚ƒEh„…

f†‚ƒ‡ˆ
(2014ZX09304307002)

uq?v
] 
£8

Š‹ŒShqɧÓÓ5©ÊÔ6…

Shq789}ij
,Tel:(010)57833097,Email:jxue@impladaccn

?v‹Œ
] 
G}

Õij¦

Š‹ŒShÓ5ij
,Email:wyjgotobd@163com
úûüýþÿ©!#­®¦$%˜$þÿ&¿…†
G}
1,
£8
1,
¤¥
1,
d>„
2,
¢¦§

(1.
SJeñfñg lm:;eñg hÁé}ijk

lm
100193;
2.
SJ<=h=>?ijg

lm
100050)

wx
] 
…†úûüý¦$%˜$Äþÿ&¿ž

é$%˜Íw) ­ËZ$ÄÍwHèü°Ÿ/&×¼

“°}J
B.#

ÿ¶#

ùPÌԄõ

O’„õa

Y±è

;u

Š

ÞùP2,ž
2h,1,2,3,4,5,7,9,11,13,15d,
“Ž&[

bcÃQR¥©!#¶}J&[‘n©!

ä+

bcÄ$%˜$úûüý©!#

¦

YÒU‰‘‚ÍúûüýÉ
”˜‘¦
764%~869%,RSD

11%,
¦
5~500μg·L-1§¹©ÙÞ,OH2þ©!«v;}JB.Tþÿ&¿–
éO’„õ
C=59922e-0338t,
ÌԄõ
C=15369e-031t,
þÿ&¿OH[/&盜ž

2,„–}é
209~224d。
bü¦­®mË}ˆÌԄõùPúûüýŸ

cª“˜“kJƒ
7d,
çD$%˜,XÍw


yz{
] 
$%˜

úûüý

þÿ&¿

2,Íwü°

2,„–}
Studyofdeltamethrindetectionmethodanditsresidual
dynamicsinLoinceraeJaponicaeFlos
WANGYujie1,XUEJian1,GUYan1,JINHongyu2,MAShuangcheng2
(1.InstituteofMedicinalPlantDevelopment,ChineseAcademyofMedicalScience&
PekingUnionMedicalColege,Beijing100193,China;
2.NationalInstitutesforFoodandDrugControl,Beijing100050,China)
[Abstract] ThispaperreportstheresidualdynamicsofdeltamethrinanddetectionmethodinLoinceraeJaponicaeFlostoprovidesci
entificbasisforsafeandappropriateuseofdeltamethrinAfieldexperimentwasconductedinFengqiu,HenanProvinceChinaThe
fieldplotsweresprayedwithdeltamethrinattherecommendeddoseandahighdose,respectively,andacontrolwassetup,totalybe
ing3treatmentswith3replicationsTheflowerswerepickedat2hours,1,2,3,4,5,7,9,11,13and15daysafterpesticideap
plicationandthendriedTheresidueofdeltamethrinwasdeterminedbygaschromatographymethodwithelectroncapturedetectorfor
theabovesamplesResultsshowedthatrecoveriesofdeltamethrinrangedfrom764% to869%,andtherelativestandarddeviation
wasbelow11%,Linearitywasobservedoverarangeof5500μg·L-1withcorelationcoeficientwas09992Theestablishedmeth
odmeetstherequirementsofpesticideresidueanalyticalmethodsThedegradationofdeltamethrinfolowedthefirstorderdynamics
TheresiduedynamicequationofthehighdoseandrecommendeddosedeltamethrinwereC=59922e-0338tandC=15369e-031tre
spectively,andthehalflifeofdeltamethrininLoinceraeJaponicaeFloswas209224days,whichindicatesthatdeltamethrinisan
easilydegradablepesticideItisconcludedthatdeltamethrinshouldbeusedinaphidsoccuringperiodandthesafetyintervalwasmore
than7daystoensurethesafetyofLoinceraeJaponicaeFlosconsuming
[Keywords] detalmethrin;LoinceraeJaponicaeFlos;residualdynamics;safeuseofpesticides;halflifeofpesticides
doi:10.4268/cjcmm20160811
·5341·
2016
y

z Ó
41
âÓ

}
Vol41,No.8 April,2016
  
$%˜æ©°ÄoE,X›[

¦,ȕ–$
­®3Q;
[1]。
’Ë…m×

úûüý¯é[,#
®„¶­®:BÞȬ

¦2¯ÉrZúûü
°

fúûüýÇÞCõü°2,

oõ«¯úûü
ý+y±¥ðÙ=¯°

éD®¦$%˜rÄ°
,Íw

…†®¦$%˜rÄþÿ&¿Ùµ£«

øù

µBúûüýÄþÿ&¿k¬
[24],
fñbm
צ$%˜ËZ$ü°ÄQ©…†

uɠҡ}
JB.#¶úûüý¦$%˜$Äþÿ&¿‘n
ó…†

bcÃQR¥#ñ¶$%˜$úûüýþÿ
õ‘n©!

åþÿ&¿ñŸåÍwü°bü

é
®¦$%˜rÄÍwü°Ÿ/&×¼

¶±!2,
¦®x,X$ÄÍwü°òA:B`{d<

1 
XL
11 
/B,X
u½.&[U}JB.â

’$%A&
®,°ÈɅ†V!u“…†Gd!é*+&ÈÉ
*+ċŒ˜°

$%˜
)。
12 

}F

zª
(60~90℃)、¯
ª‘éµî7

2
3_gj

™²«éR¥7
(FisherScientific),
úû
üý¶#[
(100g·L-1,
2`1M,é&…)©
V

/<
:GSB0523102008);
±ê´²Ë
(Fluca
D
E

‘Áµ§
,60~100
ø
,650℃
$Ì_
4h,
âê“
130℃
äZ$k
5h,
™B¦Ò¶ÃċŒÃ$

•{%‘

Ì_žÄ±ê´²Ë$:S‘i
2%
Ä
Âé‚

¦frS&ÃrS&
1h,
ƒž•{

13 
/B,„
úûüý

Q[

³#Û
,25g·L-1
Ÿ
,´
ª¯É&

$%

BCDE

14 
ÚÃ
Agilent7890A
ÃQR¥Ú

U-¡â¨©Ã

Û%ÍÜÝDE
;SB2500DT
NvjhwÚ

£jß
ŸËÉ&(âJBCDE

2 
#
21 
}JB.
}JB.¦À9e텵‘n

B.F€¦í
…µñ’ˆKÞc

$%˜[,éo)˜

ÍF,
È

(¶Þ

È`o:[%

LT–yË

ncš
90cm,`

75cm,
×x6æ
60~80cm,
×O
50~60cm。
q$€ š


(1
¶≈667m2),¥¼
ny/t7882004“
2,þÿB.‚ô
”[5]
½P

ü°
25
g·L-1
úûüý

Q[

³#Û

Ÿ

ˆ¶#

Ì
Ԅõ
(75g·hm-2)
»O’„õ
(225g·hm-2)

Y±è

|Y±è

Y;u:J

B.:J9Ë
15
m2(3m×5m),
|:Jš$%˜
18` ,
|:JJÿ
Ļn
3m,
ˆ½p“rÿ±2,

‘=Äù·¦|
[:JÄÈ`r

µeÞP,ž
2h,1,2,3,4,5,7,
9,11,13,15d
¦|:J8/ù#“Ž$%˜&[š
100g,40℃
¯‰“
60℃,
䋱è
20h
ž
,-20℃
¶Z™B

22 
&[©!
221 
R¥Ïp
 
ÍÜÝ
HP5
zõ)5*ˆ
(032mm×30m,025μm);U-¡â¨©Ã;öÃ
éO7ëÃ
(>999992%);
‘&Á‰r
250℃,
Ò
µõ‘&
;¨
©Ã‰r
300℃;¯
‰–ó

·‰r
150℃,
k
3min,
ç
10℃·min-1
ÄMr¯‰“
270℃,
k
15min;
åõÎ!

õM
1mL·min-1;
‘&õ
1μL;£#!õ。
222 
&[NPıì
 
]+ $%˜‡¢
20g(
•

<=

Þ
100mL
:MLÚX$

‘i}
F
30mL
NvŸ 
15min,
‰ž

••

&[þý¬
‘i}F
20mL
NvŸ 
15min,
;u

Š

‰ž

••

HñVB•P
。40~45℃
‚ãU“”“
¡‹

“”P¸i°
10mL
zªÑl•Ä¾¿R
¥ˆ
(12mm×250mm),
R¥ˆ8ĹLqr“À
׊éf‚ÀçÅ
2g、
x
2%
‚±ê´²Ë
4g、
f
‚ÀçÅ
2g。
°zª
(60~90℃)¯
ª
(4∶1)
O
HNP
25mL


”Žw‰P

Þ
40~45℃
™Æ
“”“¡‹

þý°zª
(60~90℃)
Nœâê
“
5mL
:MB*$

!“
3mL,


223 
¶#[NPıì
 
 úûüý‚NP
(100g·L-1)1mL
Þ
10mL
ºRõX

‘R¥7™
²«“ˆr

T
10g·L-1
NP¯é°PBÞ
-20℃
¶Z

 ã°P
1mL,
‹Œ
100
’T
100
mg·L-1
¶#[NP

3 
äÔµî
31 
úûüýxõ©!#bc
311 
Ÿ N„­»_#€†
 
¶Þ$%˜$
úûüýŸ N„€†

¶®Nœr–ÞÄN„}
F

»^ak¬ÄË,N„
[¯
ç¯ý

zª

z
ª

}F
(4∶1)][68]
‘nÜ9

ä+}F
、¯
ç¯ý

zª

}F
(4∶1)、
zª¯éŸ N„¶
500μg·kg-1‰‘&[Ÿ É”˜×Šé836%,
·6341·
ž|†Ö

úûüýþÿ©!#­®¦$%˜$þÿ&¿…†
623%,512%,413%。
}FMéuB.Ä
Ÿ N„

u½.a¼B‚#
NY/T16032008[8]

»_!

m×»_¬ÒÊ

@••–Ë,Q[


Å׈

±ê´²Ëˆ

$¹_½ˆ

»È
¹¾¿R¥ˆ
(2%
±ê´²ËÔ$¹_½OH

»_¬

m×Ë,R¥ˆ¶$%˜‘B–ÞÄ»
_¬

ÜãT’©Êu

]N۠
2%
‚±ê´²
˹?ˆ

¹LÈríÀé
2g
f‚ÀçÅ
,4g2%
‚±ê´²Ë
,2g
f‚ÀçÅ

»_¬lq
1,
’•±ê´²Ë»_ž

q

$

»



úû
üýåCøž‹HCΐ

קø›±

A.
¶#[
;B
»_ù$0&[
;C
»_ž$0&[
;1
úûüý

q
1 
$%˜$úûüý»_¬
GC
q
Fig1 Gaschromatogramofthepurificationefectofdelta
methrininLoinceraeJaponicaeFlos
312 
úûüý©!#Ü9
 
§¹ò9


P‹ŒÊôõ“rµeé
5,10,20,50,100,500μg
·L-1
Ù¯¶#[NP

µe‘&
1μL,;u2Š,
çôõ“réÔ¤

C9Ë˵^饤

§¹
Éʱè

Éʖé
Y=58474X-30051,
Q
©Ù=
R2=09992。
e¦
5~500μg·L-1úû
üý“rÔC9˧¹©ÙÞ

ÚÃÄ]+rԋ?r

 
01mg·L-1
‚
NP;u‘&

Š

ˆ#
3d
‘n
GCECD
©!


TúûüýxõÄ]+r
RSD。
çv‘•
(S/N)
é

©úûüý¨åC
(LOD);
çv‘•
(S/N)
é
10
©!#Ä!õC
(LOQ)。
äøH

{8]+

RSD

28%,
{J]+ré
56%,
OH©
!«v

úûüý¨åCé
1μg·L-1,!õCé5
μg·L-1。
#‚$r»]+r

]+ $0&[
2g,
µe]+‰‘úûüý¶#[NPT
500,200,
50μg·kg-1úûüý‰‘&[,ˆ 222ÍÀŸ
 

»_

;u

Š

©C9ËñDMxõ

Tx
‰‘“rɔ˜­]+rl+
1。3
Y‰‘“rÉ
”˜‘¦
764% ~869%,
]+r

ç
RSD
D

:
Þ
11%,
OH2þ©!
[5](
ɔ˜¦
70% ~110%,
RSD<15%)
­u½.«v

+
1 
$%˜$úûüý‰‘É”˜­]+r
(n=5)
Table1  Theaccuracyandprecisionofdeltamethrinin
LoinceraeJaponicaeFlos(n=5)
‰‘‚Í
/μg·kg-1 ɔ˜/% ͑^/% RSD/%
500 849 869 58
850
805
916
924
200 795 811 50
822
844
846
749
50 871 764 11
689
822
703
723
32 
$%˜$úûüýþÿ&¿
ˆ
21
‘n}JB.

“Ž&[
99
Y

ˆ
22
V{#¶&[‘n©!

¶#:J&[fúûü
ý¨å

uB.ÿDÄO±

Y“rúûüýþÿ
õl+
2。
ç“&OJéÔ¤

$%˜$úûüýþÿ
õ饤á±$%˜$úûüýþÿ&¿â§l
q
2。
¥¼$%˜ &OJ
(t/d)
»®úûüýþÿõ
(C/mg·kg-1),
RHåO’„õ»ÌԄõ±èþ
ÿ&¿–µeé
C=59922e-0338t(R2=09932),
C=15369e-031t(R2=09922),
þÿõ1OJ½
`=©Ù

OH[/&盜Î!

7Ô^a
k¬úûüý¦®x¯É
[4,6910]
rěœ&¿


·7341·
2016
y

z Ó
41
âÓ

}
Vol41,No.8 April,2016
+
2 
P,žÒUOJ$%˜$úûüýþÿõ
(珋x±s,
n=3)
Table2 TheresiduecontentofdeltamethrininLoinceraeJa
ponicaeFlosaftersprayingpesticide(珋x±s,n=3)
P,ž!=
/d
úûüý2,þÿõ
/mg·kg-1
ÌԄõ±è O’„õ±è
01 16±0049 67±059
1 12±011 43±040
2 093±0092 29±062
3 053±011 20±041
4 036±0043 15±027
5 031±0034 096±016
7 019±0036 063±013
9 011±0030 027±0096
11 0056±0015 014±0011
13 0026±00046 010±0033
15 <LOD 0031±00064
q
2 
$%˜úûüýþÿ&¿â§
Fig2 Thecurveofresidualdynamicssprayinghighdoseof
deltamethrin
@•–Õçå

ùPO’„õ»ÌԄõ
úûüý¦$%˜$„–}µeé
205,224d,
ù
P
15d
›œ
98%
çr

[—„–}:Þ
30d
Ä
ÇÞt›œ2,
[11],
Ø_úûüýÇÞt›œ
2,

4 
ºÒ
41 
ÂÃ$%˜rúûüýþÿÄØF
uB.

Y±èT„–}:Þ
25d,


z$¾¦À9í…B.TÄä

fæIP
,OJŸùÉö±

ô+h(„–}

@£$%
˜Ä,È+r

ù,!

!ÃáÎIV¿ÖA+Â
Ãþÿõ

42 
úûüý¦$%˜rÄÍwü°bü
ÍwJƒ}æ`¯É]ž[ŠP,c”âOV
XJƒOJ

æȯÉ]ž[Šù,žTþÿõ›
T]oþÿCõ
(MRL)
ç8VXÄ]3JƒO
J
[12]。
]ž[Šù,Ԕâ›J£ßoÞÍwJ
ƒ}

çÕÍwVW

øùoNB$%˜$úûüýÄ]oþÿCõ
‚

\%%G‚

œ[Íw%G‚œ[$2
,]oþÿCõ
GB27632014”[13]
$«v

úûü
ý¦ºé$]oþÿCõé
10mg·kg-1,
¦˜G
À­˜Á­$]oþÿCõé
05mg·kg-1,

GÀ­é
02mg·kg-1。
Qç]QÄ4éÀ­$
Ä
02mg·kg-1
éÐ܁‚

u…†$

ùPÌÔ
„õ
(75g·hm-2)
2,
7d
ž

$%˜$Äþÿõ
ÕXT_‚

$%˜¦y5

À9ªZJē˜
}[—æ

z$¾

Ø_bü“˜ù­®mËOù
Púûüý

“°ùÂP,Ä#

ùP„õé
75
g·hm-2,
ÍwJƒ}é
7d,
T]ž[ŠP,cª
“˜“k
7d
çr

A°æeI

z

<ù,

]
^

z
12
<\ö~“˜

IP,õc‘P
,Š=c‘ôQêh(Jƒ}


~=€

[1] 
Ã%˜

ÄûÜ

ÙCy

,°ÈÉ$%˜Á®3,G­hH
μ
[J].
 ´®k
,2008,26(3):56.
[2] 
ž²

5<˜

ž<

Ö

úûüý¦Å-rÄþÿ&¿
…†
[J].
y52`ok
,1989,20(3):83.
[3] 
#

Æ 

ᛛ

Ö
.25%
úûüýŸ¦o0­rÄþ
ÿΜ&¿…†
[J].
‰p®k

Èn&Ò
,2011,6
(2):40.
[4] 
h0?

ߟÇ

žÊp

‚˜P°úûüýÄþÿõ­þÿ
&¿…†
[J].
ZA®k
,1987,8(4):277.
[5] NY/T7882004
2,þÿB.‚ô
[S].
23

$%2`åÒ
a
,2004.
[6] 
kbÈ

§7„

:f›

Ö

³³É

úûüý

LÊÈûüý¦
èËrÄþÿ&¿
[J].
š¯Ék
,2011,32(5):951.
[7] 
h$C
,¨
G:

/¤

Ö

ÃQR¥#©!‚Z[$úû
üýþÿõ
[J].
¾¿2,
,2011,33(1):47.
[8] NY/T16032008
À­$úûüýþÿõÄ©!ÃQR¥#
[S].
23

$%2`åÒa
,2008.
[9] 


–,R­®üýG2,¦Ì$Äþÿ›œ­®ÂÃ
ØF…†
[D].
§

K22<&(o
,2009.
[10] 
hó~

:²

͒

úûüý¦ÎÏrþÿ&¿Ä…†
[J].
op2`ok
,1982,8(2):93.
[11] 
Ƭ×

2,M,ºè…†
[M].
23

$%M,&å
Òa
,1999:78.
[12] 
èmÊ

=

2,ÍwJƒ}­®*腆
[J].
2Z[
ôõÔÍw
,2013(5):5.
[13] GB27632014“
œ[Íw%G‚œ[$2,]oþÿCõ

[S].
23

$%‚åÒa
,2014.

‚-0
 
‘’

·8341·