OMB First to Final Action Recommendation Checklist 11-12-18

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Group

Start time, min

Monitored ion transitions, m / z

Dwell time, ms

1 2 3 4 5 6 7 8 9

14.76 15.87 18.06 19.26 20.07 21.87 22.60 23.59 26.71 27.88 28.96

306/264, 306/206

50 50 50 25 50 50 50 50 25 50 50

177/127, 177/101, 200/199, 183/102 173/145, 173/109, 238/166, 238/96

230/154, 230/111, 287/272, 287/242, 267/252, 267/93

290/233, 290/125 353/282, 353/263

359/331, 359/303, 318/248, 318/246

335/303, 335/173, 318/248, 318/246, 283/96, 283/255 148/105, 148/79, 408/363, 408/59, 237/208, 237/182

10 11

266/246, 266/218, 181/166, 181/165

341/185, 341/183

( 10 ) Ion spray voltage .—4000 V. ( 11 ) Dry gas temperature .—350°C. ( 12 ) 'U\ JDV ÀRZ UDWH ² / PLQ

F. Extraction and Cleanup Procedure (a) Sample extraction.— ( 1 ) Weigh 5 g dry tea powder (accurate to 0.01 g) into an 80 mL centrifuge tube. ( 2 ) Add 15 mL acetonitrile. ( 3 +RPRJHQL]H DW USP IRU PLQ ( 4 &HQWULIXJH DW î g for 5 min at room temperature. ( 5 7UDQVIHU WKH VXSHUQDWDQW LQWR D SHDU VKDSHG ÀDVN ( 6 5H H[WUDFW WKH VDPSOH ZLWK P/ DFHWRQLWULOH KRPRJHQL]H FHQWULIXJH DQG FRPELQH WKH VXSHUQDWDQWV IURP WKH WZR H[WUDFWLRQV ( 7 &RQFHQWUDWH WKH H[WUDFW WR DSSUR[LPDWHO\ P/ LQ D URWDU\ evaporator (or TurboVap) in a 40°C water bath. ( 8 3ODFH D SHDU VKDSHG ÀDVN LQ WKH YDFXXP PDQLIROG ( 9 ) Mount a Cleanert TPT cartridge onto the manifold. ( 10 $GG DQK\GURXV VRGLXP VXOIDWH DSSUR[LPDWHO\ FP RQWR WKH &OHDQHUW 737 SDFNLQJ PDWHULDO ( 11 $GG P/ DFHWRQLWULOH±WROXHQH Y Y WR DFWLYDWH WKH cartridge. ( 12 6WRS WKH ÀRZ WKURXJK WKH FDUWULGJH ZKHQ WKH OLTXLG OHYHO LQ the cartridge barrel has just reached the top of the sodium sulfate SDFNLQJ ( 13 'LVFDUG WKH ZDVWH VROXWLRQ FROOHFWHG LQ WKH SHDU VKDSHG ÀDVN DQG UHSODFH ZLWK D FOHDQ SHDU VKDSHG ÀDVN (b) SPE cleanup .—( 1 /RDG WKH FRQFHQWUDWHG H[WUDFW IURP F ( a )( 7 ) into the conditioned Cleanert TPT cartridge collecting WKH HOXDWH LQWR WKH FOHDQ SHDU VKDSHG ÀDVN ( 2 5LQVH WKH SHDU VKDSHG ÀDVN WKDW FRQWDLQHG WKH FRQFHQWUDWHG H[WUDFW ZLWK î P/ DFHWRQLWULOH±WROXHQH Y Y

( 13 ) Monitored ion transitions, collision energies, and fragmentation energies for the 20 pesticides and chlorpyrifos methyl are shown in Table 2014.09F , and SRM acquisition parameters by /& 06 06 IRU WKH SUHFXUVRU DQG SURGXFW LRQ WUDQVLWLRQV PRQLWRUHG are shown in Table 2014.09G . (d) Homogenizer ²5RWDWLRQDO VSHHG KLJKHU WKDQ U PLQ (report also in g IRUFH XQLWV 7 % -DQNH .XQNHO 6WDXIHQ *HUPDQ\ RU HTXLYDOHQW (e) Rotary evaporator ²%XFKL (/ )ODZLO 6ZLW]HUODQG RU equivalent. (f) Centrifuge ²&HQWULIXJDO IRUFH KLJKHU WKDQ î g = % +HUP/H $* *RVKHLP *HUPDQ\ RU HTXLYDOHQW (g) Nitrogen evaporator ²(9$3 2UJDQRPDWLRQ $VVRFLDWHV ,QF 1HZ %HUOLQ 0$ 86$ RU HTXLYDOHQW (h) TurboVap ²/9 (YDSRUDWLRQ 6\VWHP &DOLSHU /LIH 6FLHQFHV +RSNLQWRQ 0$ 86$ RU HTXLYDOHQW (i) 9LVLSUHS SRUW ÀDVN YDFXXP PDQLIROG ²56 683(/&2 8 6LJPD $OGULFK 6KDQJKDL 7UDGLQJ &R /WG See Figure 2014.09 . (j) Variable volume pipets ² ȝ/ ȝ/ DQG P/ (k) Balance .—Capable of accurately measuring weights from 0.05 to 100 g within ±0.01 g.

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Mobile phase A (0.1% formic acid in water, %)

Mobile phase B (acetonitrile, %)

Step

Time, min

)ORZ UDWH ȝ/ PLQ

0 1 2 3 4 5 6 7

0.00 3.00 6.00 9.00

400 400 400 400 400 400 400 400

99.0 70.0 60.0 60.0 40.0

1.0

30.0 40.0 40.0 60.0 99.0 99.0

15.00 19.00 23.00 23.01

1.0 1.0

99.0

1.0

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