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7/28/2019 2010 Pang Tea Protocol-2
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HighHigh--Throughput Analytical MethoThroughput Analytical Metho
an muan mu -- n s o es ue esn s o es ue es
by GCby GC--MS, GCMS, GC--MSMS
AOAC CollaborativAOAC Collaborativ
AOAC Study DireAOAC Study DireAcademy of Chinese IAcademy of Chinese I
Email:qhdciqgfpEmail:qhdciqgfp
Call for Voluntary CollaboratorsCall for Voluntary Collaborators
Priority Project of AOAC INTERNATIONAL (2010)Priority Project of AOAC INTERNATIONAL (2010)
Nov. 27, 2010)Nov. 27, 2010)
for Determination of multifor Determination of multi--ClassesClasses
c es an em ca o u an s n eac es an em ca o u an s n ea
MS and LCMS and LC--MS/MSMS/MS
Stud Protocol DraftStud Protocol Draft
tor: Guotor: Guo--Fang PangFang Pangspection and Quarantinespection and Quarantine
[email protected]@yahoo.com.cn
1
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3. Analytical procedures3. Analytical proceduresCentrifugalize
Concentration
Clean-up
Homogenize at 13500r/min for 1min;
Centrifuge at 4200r/min for 5min;Concentrate to ca 1mL at 40;
The key control points
Elute by gravity for clean-up;
Concentrate to ca 0.5mL at 40;
Evaporate to dryness with nitrogen gas at 3
Filter through 0.2m membrane
Concentration Concentration
Eva
GC-MS-SIMHomogenize
GC-MS-MSSampler vial
Determine
LC-MS-MSporate with nitrogen
4
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3. GC3. GC--MS(GCMS(GC--MS/MS)&LCMS/MS)&LC--MS/MS AnaMS/MS Ana
5g tea sample
Add 15 mL acetonitrile
Homogenize at 13500r/min for 1min, and centrifuge at 4200r/
supernatants are taken, while the dregs are re-extracted and the
Cleanert TPT Cartridge(2g,12mL) or Envi-Carb/PSA(0.5g/0.5g,6mL)
mL acetonitrile+toluene(3+1), concentrated to about 0.5 mL
Add IS Heptachlor epoxide for GC/MS-SIM, GC/MS/MS or Chlorp
Evaporate to dryness with nitrogen at 35
Make up to 1.5 mL with hexane
GC/MS
Determination
(490 Varieties)
-
ysis programysis programwould like to
remind all the
participants, as a
binding rule for
voluntary
participation: thisinter-collaborative
study is a unifiedin for 5 min before the
extracts are combined and
for clean up. Elute with 25
action for all the
collaborators from
different countries
all over the world,
rifos-methyl for LC-MS/MS.
ake up to 1.5 mL with
an eac s ep
involved in the
experiment
including reagents
and testin
LC-MS/MS
Determination
(448 Varieties)
materials shall notbe altered or
replaced without
the prior consent
5
- .
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4. Shrunken AOAC collaborative stu4. Shrunken AOAC collaborative stu
ItIt
ersonerson
4.14.1 20 pesticides for GC20 pesticides for GC--MS(GCMS(GC--MS/MS) and LCMS/MS) and LC--MS/MSMS/MS
NoGC-MS LC-MS/MS
Pesticides MRL/ (g/kg) Pesticides MRL/ (g/kg)
onon hunhun
anan altealte
andand twtw
res ecres ec
1 2,4'-DDE 200 acetochlor 10
2 benalaxyl 100 benalaxyl 100
3 bromophos-ethyl 100 bensulide 30
4 bromopropylate 100 butralin 20
5 chlorfenapyr 50000 chlorpyrifos 100
bebe invoinvo
20 pe
(G
6 diflufenican 50 clomazone 20
7 dimethenamid 20 diazinon 20
8 fenchlorphos 100 ethoprophos 20
9 picoxystrobin 100 fenazaquin 10
prmcar u o an
11 pirimiphos-methyl 50 imidacloprid 50
12 bifenthrin 5000 indoxacarb 50
13 propyzamide 50 kresoxim-methyl 100
14 pyrimethanil 100 phenothrin 50
classified p
comp
Carbamate
Organophospho
15 Quinoxyfen 50 picoxystrobin 100
16 tebufenpyrad 100 pirimiphos methyl 50
17 tefluthrin 50 propoxur 100
18 tolclofos-methyl 100 tebufenpyrad 100
19 trifluralin 100 triadimefon 200
Organohaloge
Pyrethroid
Organonitroge
* Indicates the pesticides to be determined by both GC-MS (GC-MS/MS) and LC-MS/MS
20 vinclozolin 100 trifloxystrobin 50Other
dy protocoldy protocol
illill bebe extremelyextremely difficultdifficult inin termsterms ofof resources,resources, timetime andand
nelnel forfor eacheach artici antartici ant toto or anizeor anize aa collaborativecollaborative studstud
determinationsdeterminations
dredsdreds ofof pesticides,pesticides, soso AOACAOAC InternationalInternational hashas proposedproposed
rnativernative shrunkenshrunken protocol,protocol, whichwhich isis toto selectselect twotwo teasteas
methodsmethods ofof GCGC--MSMSGCGC--MS/MSMS/MS andand LCLC--MS/MSMS/MS forfor aaiveive determinationdetermination ofof 2020 esticidesesticides totalintotalin 4040 esticidesesticides toto
lvedlved inin thethe collaborativecollaborative studystudy..
ticide classes for GC-MS
-MS/MS) detemination
20 pesticide classes for
LC-MS/MS detemination
er chemical
sitionsclassified per functions
1 Acaricide 2
rus 4 Herbicide 4
classified per functionsclassified per chemical
compositions
Carbamate 2Plant growth
regulator1
n 2 Insecticide 8
2 fungicide 6
n 9
Organophosphorus 5 Acaricide 2
Organonitrogen 12 Herbicide 3
Other 1 Insecticide 8
6
2 ungicide 6
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4. Shrunken AOAC collaborative stu4. Shrunken AOAC collaborative stu
Each sample is only sufficient for one test, in other words,
4.2 Each participating laboratory makes a determi
,
Director will emphasize again that this collaborative study
of these 16 collaborative study samples are as follows:
*each sample shipped will be determined later.
dy protocoldy protocol
each participant will have only one testing opportunity for
ation of a total of 16 collaborative study samples.
. ,
ust be dealt with full focus and attention. The compositions
TheThe concentrationconcentration rangerange ofof 2020 targettarget pesticidespesticides isis1010ug/kgug/kg--22..00mg/kgmg/kg equivalentequivalent toto 11MRLMRL--55MRLMRL..
orti ieorti ie samp essamp es anan pestici epestici e ageage samp essamp es arearedesigneddesigned inin YoudenYouden Pair,Pair, withwith twotwo samplessamples forfor oneone pairpair
andand thethe differencedifference ofof thethe concentrationconcentration ofof thethe targettargetpesticidepesticide isis aboutabout 55%%..
7
,
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5. The flow chart of the AOAC collabor5. The flow chart of the AOAC collaborative studative stud
Excel Worksheet
8
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--
(1)For Pre(1)For Pre--collaborative studycollaborative study
20 pesticide mixed standard stock solutions: 2 ampoules
(1.0mL X 2, 1 spare aged). Internal standard stock solutions: 2 ampoules (1.0 mL X 2,
1 spare aged).
(200g x 2).
Examination sample materials:
3 ampoules of fortified solutions (0.5mL x 3) for preparationof examination samples. 3 bags of green tea blank samples (5.0g x 3) for preparationof examination samples. 3 bags of woolong tea aged samples (5.0g x3).
(3)For Qua(3)For QuaQuality control standard stock solutions:
for checkin the instrumental sensitivit an
(2)For Collaborative study(2)For Collaborative study
2 ampoules (1.0mL x 2, 1 spare aged) of 20 pesticide mixed
standard stock solutions for establishing at least 5 point matrix-
matched internal standard calibration curve.
2 ampoule (1.0mL x 2, 1 spare aged) of internal standard stock
.
10 ampoules (0.5mL x 10) of fortified solutions for preparation of
fortified samples.
10 bags of tea blank samples(5.0 g x 10): No. 01-No.05 is green tea;
No.06-No.10 is woolong tea for preparation of fortified samples. 6 bags of aged tea samples (5.0 g x 6): No.11-No.13 is green tea;
No.14-N0.16 is woolong tea.
1 bottle of green tea and woolong tea blank samples each (200g x
2) for preparation of matrix-matched internal standard calibration
mixed solutions.
lity Controllity Control2 ampoules (1.0mL X 2, 1 spare aged), usedstabilit .
9
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SteSte --II PreII Pre--collaborative studcollaborative stud
Step-II The significanceBecause of the complexity of tea mat
research and the nature of technology in
,
well explained in the remarks of AOAC S
Krystyna McIve pre-collaborative stud
Study Director reminds everyone here once again: F
participant will have only one testing opportunity, whishot. However, the practice samples that Study Dir
rehearsal in order to meet the objective of dexterous
rices, the magnitude of content of thevolved, this collaborative study is by no
-
r. Director, Stakeholder Communications
by the collaborators to ensure the.
r each of these 16 collaborative study samples, each
ch means success or failure is determined by just onector provides shall be sufficient for full practice or
astery of the key control points. We hope that you will
-
10
.
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StepStep--II PreII Pre--collaborative studycollaborative studyStep-II Practice stageThis collaborative study adopts internal standard
respectively 20,50,100,200 and 300 uL pesticides mixe
internal standard working solution for GC-MS or GC-Msolution for LC-MS-MS) before mixing uniformly.
Use nitrogen blow to dryness, dissolve residua by 1.5- , ,
calibration mixed solutions. Establish 5 point matrix-mpractice spiked recovery test
Each lab use blank tea samples and 20 pesticidesrecovery test at 1MRL and 5MRL levels on ones own. Istudy, he may undertake examination samples.
At least 5 point matrix matched internal standard calibr Recoveries fall within 70-120% with RSD
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SteSte --II PreII Pre--collaborative studcollaborative studStepStep--IIII examination stageexamination stage Preparation and determination of fortified samples for Green Tea: add thr
Director into three 80mL centrifugal tubes with the same serial numbers,No.3 upright stand in front of the centrifugal tubes with the same serial n
bottom before opening the bottle and add all the fortified solutions into thetimes separately and add the washings into the centrifugal tube. Wait for 2sample preparation per 6.1 Extraction and 6.2 Cleanup in the AOAC collasolutions and establish internal standard-matrix-matched calibration curve
oo ong ea age samp es o. - o. are prepare per e me o as mensolutions and establish internal standard-matrix-matched calibration curve
Verifying the test results against the following three methods:1) whethercorrect; 3) mass spectrum resolution is checked if ion abundance complies
The instrument analytical parameters of
AOAC collaborative study
Determination resul
examination samples
Study Director will provide ample feedback of the study res
-
1-3, mass spectrum chromatographs and raw data, Study
examination results within 48 hours for collaborators to dec
Serial Nos. No.01 No.02 No.03
The Corresponding Serial Numbers of Centrifugal Tubes, Blank Samples
and Fortified Solution Ampoule Bottles
ee bags of Green Tea blank samples No.1, No.2 and No.3 shipped by Study
. . .
Blanks samples No.01 No.02 No.03
Fortified solutions No.01 No.02 No.03
and place three ampoule bottles contained fortified solutions No.1, No.2 andumbers. Wait till solutions at the top of the ampoule bottle flow down to the
hree centrifugal tubes with the same numbers. Rinse the ampoule bottle three0min until the solutions are fully absorbed by the sample before undertakingborative study. In the meanwhile, prepare 5 portions Green Tea matrix blankused for quantification of Green Tea fortified samples.
one a ove. n e meanw e, prepare por ons oo ong ea ma r x anfor quantification of Woolong Tea incurred samples.the retention time is within the time window; 2) whether integration line iswith requirements of EU standard or AOAC standard.
s of practice
by GC-MS-SIM orDetermination results of practice
examination samples by LC-MS/MS
ults to each collaborator. Upon reception of Excel worksheet
12
Director will promptly reply to each collaborator regarding
ide whether to continue with the collaborative samples.
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SteSte --II PreII Pre--collaborative studcollaborative studStepStep--IIII Acceptance criteria for preAcceptance criteria for pre--colcol -
standard calibration curve R2
0.995 for GMS (GC-MS/MS) or LC-MS/MS.
-RSD
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--StepStep--IIIIII Drawing at least 5 point matrixat least 5 point matrix--matcmatc
ThisThis collaborativecollaborative studystudy adoptsadopts matrixmatrix--matchedmatched inin
GCGC--MSMS--SIMSIM andand GCGC--MS/MSMS/MS usesuses HeptachlorHeptachlorchlorpyrifoschlorpyrifos--methylmethyl asas internalinternal standardstandard..
repara onrepara on proce uresproce ures oo po npo n ma r xma r x--ma c ema c ePreparePrepare 55 portionsportions ofof GreenGreen TeaTea andand WoolongWoolong2020,,5050,,100100,,200200 andand 300300 uLuL pesticidespesticides mixedmixed stanstan
workingworking solutionssolutions beforebefore mixingmixing uniformlyuniformly..,,
acetonitrileacetonitrile:: waterwater ((33::22)) (LC(LC--MS/MS),MS/MS), mixmix thoroughthoroughstandardstandard calibrationcalibration mixedmixed solutionssolutions.. AfterAfter detedetestandardstandard calibrationcalibration curvecurve..
From a practical view, the matrix used in calibration wsamples, i.e. Green Tea samples shall be quantified with Gcurve while Woolong Tea samples shall be quantified withwhich cannot be confused with. Matrix matched standard c
.
ed internal standard calibration curveed internal standard calibration curve
ternalternal standardstandard calibrationcalibration curvecurve forfor quantificationquantification..
epoxideepoxide asas internalinternal standardstandard.. LCLC--MS/MSMS/MS usesuses
n ernan erna s an ars an ar ca ra onca ra on curvecurve areare asas o owso ows::TeaTea blankblank samplesample solutionssolutions each,each, addadd respectivelyrespectivelydarddard workingworking solutionssolutions andand 4040uLuL internalinternal standardstandard
-- -- --ly,ly, andand prepareprepare toto bebe 55 pointpoint matrixmatrix--matchedmatched internalinternalmination,mination, establishestablish 55 pointpoint matrixmatrix--matchedmatched internalinternal
rking curve shall have to be the same as that of the targeteen Tea matrix-mached internal standard calibration workingoolong Tea matrix-mached standard calibratin working curve,libration working solutions should be prepared for immediate
14
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--Step-III Preparing collaborative fortified samples (t
Add 5 portions of Green Tea blank samples supplied by Study
.
front of the corresponding centrifugal tubes. Wait till solutions
opening the bottle and add all the fortified solutions into the centriftimes with 0.5 mL toluene and add the washings into the centrifugal
sample to form collaborative fortified samples before undertaking s
AOAC collaborative study.
Serial Nos. No.01 No.02
Centrifugal tubes No.01 No.02
Study Director specially reminds each participant: 1) a portion of fortifi
. .
Fortified solutions No.01 No.02
or on y one ana ys s. e concen ra ons o or e so u ons n eac
take special precautions to transfer them thoroughly. 2) To avoid c
concentrations or contaminations of blank samples), samples prepar
serial numbers, and the utensils for sample preparations used shall be
contamination of next sample preparation.
Step-III Aged samples are prepared per section 6-1 extractio
aking 5 Green Tea fortified samples for instance)Director Nos1-5 to a 80mL centrifugal tube with the same serial
t the top of the ampoule bottle flow down to the bottom before
gal tubes with the same numbers. rinse each ampoule bottle threetubes. Wait for 20min until the solutions are fully absorbed by the
mple preparation per section 6.1 Extraction and 6.2 Cleanup in the
No.03 No.04 No.05
No.03 No.04 No.05
ed solutions corresponding to a portion of blank samples is sufficient
. . .
No.03 No.04 No.05
mpou e o e are un nown o eac par c pan , requ r ng m or er o
oss-interference of samples (especially high concentrations vs. low
tions and determinations shall be conducted in accordance with the
thoroughly rinsed or cleansed one time after one use so as to prevent
15
n and 6.2 cleanup in the collaborative study method.
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--
Step-III GC-MSGC-MS/MSor LC-MS/
Before making determinations of collaborativsolutions to check if the instrumental sensitiviAfter com letion of testin a consi nmentworking solutions to check if the instrumental
and after.
Abide strictly by qualitative and quantitativre en on me an on a un ance o eac p
within the integration window and identified coCheck to see if the integration line of eacone peak valley to another peak valley.Collaborators shall submit to Study Directorworksheets.
MS analytical requirements
samples, use quality control standard workingy and stability have met the requirements.
f sam les, re-run the ualit control standard
sensitivity and stability are in agreement before
e requirements of the method and check thea o ensure a eac arge pes c e pea s
rrectly.
pesticide peak is selected correctly, and for
the official collaborative study results by Excel
16
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StepStep--IV Collaborators shall submit to SIV Collaborators shall submit to S
study results by Excel worksheets.study results by Excel worksheets.
The instrumental analytical parameters (quworksheet 1 of Annex B of the collaborative Determination results of Collaborative studworksheet 4 of Annex B of the collaborative Determination results of Collaborative studo nnex o e co a ora ve s u y me o
The instrument analytical parameters
of AOAC collaborative study
Determination res
study samples by G
tudy Director the official collaborativetudy Director the official collaborative
litative and quantitative ions aged), see Excelstud method.
y samples by GC-MS or GC-MS/MS, see Excelstudy method.
samples by LC-MS/MS, see Excel worksheet 5.
lts of Collaborative
C-MS or GC-MS/MS
Determination results of Collaborative
study samples by LC-MS-MS
17
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StudyStudy DirectorDirector entersenters thethe analyticalanalytical resultsresults forfor
collaboratorscollaborators intointo thethe followingfollowing Table,Table, perper thethe
ofof thethe testtest results[results[44]]..
Matrix-matched internal standard calibration curve R20.995.en ca on o arge pes c es n s co a ora ve
tea samples adopts EU Standard [2] Recoveries, RSDr and RSDR are judged per the AOAC
Guidelines for single laboratory validation of chemical
Relative intensityRelative intensity(( of base peak)of base peak) GCGC--MSMS--SIMSIM(relative)(relative) GCGC--MSMS--MS,LCMS,LC--MS/MSMS/MS(relative)(relative)
Recommended maximum permitted tolerances for relative ion intensities using aRecommended maximum permitted tolerances for relative ion intensities using a
range of spectrometric techniquesrange of spectrometric techniques
.
5050 1010 20%20%
2020--5050 15%15% 25%25%
1010--2020 20%20% 30%30%
1010 50%50% 50%50%
ConcentrationConcentration Recovery limitsRecovery limitsRepeatabilityRepeatability
(RSD(RSDrr))ReproducibilityReproducibility
(RSD(RSDRR))
10 g/g(ppm)10 g/g(ppm) 8080--115115 6%6% 11%11%
1g/g1g/g 7575--120120 8%8% 16%16%
18
10 g/kg(ppb)10 g/kg(ppb) 7070--125125 15%15% 32%32%
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. qu pmen qua ca on. qu pmen qua ca on
Instrumental sensitivity is calculated per intGC-MS-SIM1000GC-MS/MS2000LC-MS/MS500 Instrumental stability (calculated per internRetention time deviation
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8. SPE equipment qualification8. SPE equipment qualification
Based on the suggestions from experts at the community
multiresidues in tea and the two cartridges, Cleanert-TPT
8.1 Recoveries and RSD requirement
experiment was conducted at 2MRL level on the cleanup
CARb+PSA (500mg/500mg, 6mL) from seven manufacturerBestown with Cleanert-TPT for 340 pesticides (LC-MS/MS)
Woolong Tea, with the results as follows:
Evaluation of cleanup efficiencies of SPE cartridges against 340 pesticides
SPECartridge
Brands UCT SUPELCO
fillers GCB/ PSAENVI-CARB-II
/PSAelution time min 1429 1426
Elution flow ratedrop/min
before Connecting the reservoir 4055 6290
After Connecting the reservoir 83115 80120
Percentage of pesticides with recoveries between 70-120% 96.5 97.1
Percentage of pesticides with RSD
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8. SPE equipment qualification8. SPE equipment qualification8.2 De-pigmentation levels
Viewed from de-pigmentation results, Cleanert-TPT from AgelCARB-II/PSA from Supelco, Carbon/PSA from Agilent, andWaters, GCB/PSA from CNW belong to Grade III; PSA/CARB fr
(a) Fig.1 Comparison of depigmentation results from Green
In terms of percentage of the number of pesticides with rmajority of pesticides are in conformity with the acceptance The conclusion was shown as follow:
- - +,
on 183312 data from our previous 912 experiments haveefficiencies of both cartridges are of Ruggedness.
secondly, this comparative experiment of cleanup efficiencieCarbon/PSA (500mg/500mg, 6mL), in terms of recoveries a
.AOAC pre-collaborative study, they may use these cartridges
does the best, belonging to Grade I; GCB/PSA from UCT, ENVI-Carbon/PSA from Varian belong to Grade II; Carbon/PSA fromom Bestown belong Grade IV.
(b)ea (a) and Woolong Tea (b) by 8 cartridges
coveries between 70-120% and RSD
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. equ pmen qua ca on. equ pmen qua ca on
Two cartrid es are recommended for this collabTwo cartrid es are recommended for this collab1) Cleanert TPT (12 mL, 2000 mg, Agela, Tianjin1) Cleanert TPT (12 mL, 2000 mg, Agela, Tianjin
(http://www.agela.com/searchproduct.aspx?(http://www.agela.com/searchproduct.aspx?2) Envi2) Envi--Carb +PSA (0.5g/0.5g,6mL, Supelco,USCarb +PSA (0.5g/0.5g,6mL, Supelco,US
No matter which cartridge is selected, itNo matter which cartridge is selected, it isisrecommended to use Visiprep 5recommended to use Visiprep 5--port flask vaport flask vamanifold or e uivalent RSmanifold or e uivalent RS--SUPELCO 57101SUPELCO 57101--Aldrich Trading Co., Ltd), which is a solidAldrich Trading Co., Ltd), which is a solid--phphextraction equipment newly developed by Suextraction equipment newly developed by Su(http:www.sigmaaldrtch.com)(http:www.sigmaaldrtch.com)
The Supelco Visiprep 5-Port flask vacuum manifold reco
volumes of cleansing liquid (32mL). If collaborators are abl
, .
TPT cartridges can not be easily accessed in the region, Stud
rative stud :rative stud :China);China);
earch=tpt )earch=tpt )))
cuumcuumU Si maU Si ma
Solid phase Extraction Equipment
sesepelco.pelco.
mended here is that it is relatively convenient to receive big
e to solve the reception of big volume (32mL) in Cartridge
22
Director may provide necessary assistance.
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9. Checking the interference and influ9. Checking the interference and influTo prevent the interferences from reagent
reagents in the entire process of the method
and each laboratory is requested to supply
Director.
10. Avoiding cross10. Avoiding cross--interferences amointerferences amothe reagentsthe reagents
To prevent cross-interferences among the s
thoroughly cleansed 30 seconds homogenously
sample extraction so as to avoid the interfere
content from the sam les of hi h esticide cont
study.
nces from the reagentsnces from the reagents, blank tests shall be conducted on the
to confirm there are no interfering peaks,
black test TIC chromatographs to Study
g the samples and influence fromg the samples and influence from
mples, the blade of the homogenizer, after
,
with 2x50 mL acetonitrile in the same way as
ces on the samples of low or non pesticide
ent which is a ke oint in this collaborative
23
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11. Sample testing sequence requirem11. Sample testing sequence requirem
For collaborative sample testing, Study Direc
observed sequentially: before testing sample
control standard working solutions (to chec
successive injections of matrix-matched inter
concentrations from low to high 1, 2, 3, 4 anstandard calibration curve), use sample testin
num er o g per e or er o ser a num
standard working solutions 2-3 times ( to check
..
ExpertiseExpertise necessarynecessary forfor collaboratorscollaborators andand techntechn
11 SkillfulSkillful sam lesam le re arationre aration techni uestechni ues ofof eses
22)) SkillfulSkillful analyticalanalytical techniquestechniques withwith GCGC--MSMS--SS(operational(operational experience,experience, judgingjudging experiencexperienc
repairrepair experience)experience)..
rec serec se massmass spec rome r cspec rome r c reso v ngreso v ng ec nec n
entsents
or suggests that the following order shall be
s, conduct 2-3 repeated injections of quality
instrumental sensitivity and stability), make
nal standard calibration mixed solutions with
5 points (to draw an matrix-matched internalsolutions to test No.01, No.02( from small
rs an na y repea es ng qua y con ro
again instrumental sensitivity and stability).
icalical expertsexperts..
icideicide residuesresidues..
IM,IM, GCGC--MS/MSMS/MS andand LCLC--MS/MSMS/MS andand experienceexperiencewithwith troubletrouble--shootingshooting andand maintenancemaintenance andand
24
ueue oror res uares ua pes c espes c es
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..
After AOAC Pesticide and Chemical Contamin
s end two months recruitin collaborators w
countries and regions.
As soon as the collaborators are finalized,
standard solutions, fortified solutions and rel
collaborative study and official collaborative s
service. Counted from the date of shipping th
are kindly requested to finish this AOAC collabUpon reception of these collaborative material
testing materials received conform to those in
and safe and fill in the Receipt Form (see A
.
are required to finish analytical tasks of all sa
nts Committee approves this protocol, we will
rldwide aimin at 20-30 laboratories from 15
we will immediately set about preparing the
evant testing consumables, etc. used for pre-
tudy and ship them out in one lump by courier
se testing materials from China, collaborators
orative study within 3 months.s, collaborators shall immediately check if the
the packing list and if the materials are sound
nex 1), which should be emailed or faxed to
,
ples within 2 months at the latest.
25
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14. Safety measures14. Safety measures
Acetonitrile,Acetonitrile, toluenetoluene andand otherother reagentsreagents usedused inin
healthhealth.. Therefore,Therefore, itit isis speciallyspecially remindedreminded thatthat rr
o erationo eration withwith carecare inin thethe ventilatedventilated cabinetcabinet shouldshould
15. Study Directors hope, requests a15. Study Directors hope, requests a
methodmethod (GC(GC--MS,MS, GCGC--MS/MSMS/MS oror LCLC--MS/MS)MS/MS) partiparti
StudyStudy DirectorDirector requestsrequests eacheach participatingparticipating lablab8080 daysdays fromfrom receptionreception ofof testingtesting materialsmaterials anan
chromatographs,chromatographs, rawraw data,data, etcetc.. toto StudyStudy DirectDirect StudyStudy DirectorDirector promisespromisesduringduring thethe collaborcollabortechnicaltechnical questionsquestions fromfrom participantsparticipants withinwithin 4848
oo ourour eses oo e pe p ouou ..
thisthis experimentexperiment areare ofof potentialpotential hazardhazard toto humanhuman
bberbber glovesgloves shallshall bebe wornworn inin experimentsexperiments andand
bebe observedobserved..
d promisesd promises
--
cipatingcipating inin thisthis collaborativecollaborative studystudy..
ratoryratory toto concludeconclude thisthis collaborativecollaborative studystudy withinwithin
dd toto emailemail oror faxfax thethe analyticalanalytical resultresult datadata sheets,sheets,
rr himselfhimself..tivetive studystudy period,period, StudyStudy DirectorDirector willwill replyreply toto anyany
hourshours;; ForFor questionsquestions inin otherother aspectsaspects wewe willwill alsoalso
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16. References16. References
1. http://www.flworkshop.com/Community/pesticides.html
2. Document No. SANCO/10684/ 2009Method Validation and
Food and Feed
3. AOAC Guidelines for single laboratory validation of chemical
. . . . .
5. Standardization Administration of P.R.China (2008) GBT 232
residues in teaGC-MS method6. Standardization Administration of P.R.China (2008) GB/T 23
residues in teaLC-MS-MS method
7. High-Throughput Analytical Techniques for determination o
Chemical Pollutants in Tea. Part I: The Tentative Probe into
Manuscript ID-10-0008R.1)
8. High-Throughput Analytical Techniques for determination o.
(J.AOAC Int. Manuscript ID-10-0215R.1)
9. High-Throughput Analytical Techniques for Determination
Chemical Pollutants in Tea. Part III: The Evaluation of t
Multiresidues in Tea (J.AOAC Int. Manuscript ID-10-0251R.1)
10. High-Throughput Analytical Techniques for Determination
Chemical Pollutants in Tea. Part IV: Key Control Points and
the draft)
11. High-Throughput Analytical Techniques for Determination
Chemical Pollutants in Tea. Part V: Establishment of AOAC
Prediction for Detected Values of Multiresidues of Collaborati
Quality Central Procedures for Pesticide Residues Analysis in
methods for dietary supplements and botanicals
, , .
4-2008 , Determination of 519 pesticides and related chemicals
05-2008, Determination of 448 pesticides and related chemicals
f 653 multi-Classes and multi-Kinds of Residue Pesticides and
the Analytical Techniques of Multiresidues in Tea (J.AOAC Int.
f 653 multi-Classes and multi-Kinds of Residue Pesticides and
of 653 multi-Classes and multi-Kinds Residue Pesticides and
e Cleanup Efficiency of SPE Cartridge Newly Developed for
of 653 multi-Classes and multi-Kinds Residue Pesticides and
rror Analysis of AOAC collaborative Study Method (has formed
of 653 multi-Classes and multi-Kinds Residue Pesticides and
ollaborative Stud Pesticide De radation Kinetic E uations and
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ve Study Samples (being written)
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Chinese Academy of InChinese Academy of In
..
Email: qhdciqgfpEmail: qhdciqgfp
spection and Quarantinespection and Quarantine
, ,, ,
[email protected]@yahoo.com.cn
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