2010 pang tea protocol-2

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

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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

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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

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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 .

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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

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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

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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

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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

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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.

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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)


Chemical Pollutants in Tea. Part IV: Key Control Points and

the draft)


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

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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


rror Analysis of AOAC collaborative Study Method (has formed


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

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Email: qhdciqgfpEmail: qhdciqgfp

spection and Quarantinespection and Quarantine

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[email protected]@yahoo.com.cn

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2010 pang tea protocol-2

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