Phn tch acetamiprid trong go v rau qu bng k thut LC-MS/MS

Ni dung chnh.I. K thut MS-MS 1. S LC MS/MS 2. Khi ph MS-MS 3. Ngun ion ho II. Phng php phn tch. 1. Nguyn tc. 2. Quy trnh chun b mu. III. Kt qu v tho lun. 1. Ti u phng php chit mu 2. Ti u iu kin chy my. 3. Kt qu xc nh khong tuyn tnh. 4. Kt qu xc nh CV thit b, LOD, LOQ phng php. 5. Kt qu xc nh CV v thu hi trung bnh ca phng php.

1. Nguyn nhn. - Phng tr ry nu. - Thi gian tn d lu. 2. Hu qu . - nh hng xu ti sc kho. - Gy thit hi kinh t.Cng thc cu to

S LC/MS-MS

1. Bnh cha dung mi pha ng

2.Bm cao p 3.B m mu

5.Ngun

6. Khi

4. Ct tch

ion ho

ph MS

7. PC iu khin

Khi ph MS - MS

Ngun Ion ho

Ion ho ho hc p sut kh quyn APCI

CH3COONH4 H+ + Acetamiprid + H+ [Acetamiprid ]+

Nguyn tc

- D lng Acetamiprid chit ra khi mu bng hnhp dung mi. - Hot cht c pht hin bng HPLC-MS/MS Agilent 6410 Triple. - Kt qu c tnh da trn s so snh gia t s s o din tch pic mu v pic chun

Chun b mu

iu kin HPLC.1. Ct sc k Agilent RP C18 2.1x150mmx5m 2. H pha ng v chng trnh dung mi Knh A : MeOH : H2O = 2 :8 + 5 mmol CH3COONH4 Knh B : MeOH : H2O = 9 :1 + 5 mmol CH3COONH4

3. iu kin MS/MSHot cht Precursor ion Product Dwell Farg (v) ion Time (ms) CE (v)

Acetamiprid

223

126 90,1

200 200

140 140

15 5

Sc k v ph ca Acetamiprid ti 1 ng/ml+ MRM (223.0 -> 126.0) 270508013.d Abundance x10 3 3.5 3.25 3 2.75 2.5 2.25 2 1.75 1.5 1.25 1 0.75 0.5 0.25 0 -0.25 5 5.5 6 6.5 223 -> 126.0 , 126.0 Relative Abundance (%) x10 4 3.2 3 2.8 2.6 2.4 2.2 2 1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 -0.2 5 5.5 6 6.5 Ratio= 100.0

+ MRM (5.712-6.014 min, 45 scans) 2 Abundance x10 2 2.4 2.2 2 1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0

5.822 Acetam iprid

126.0

90.1100 150 200 Mass-to-Charge (m/z)

Acquisition Time (min)

Acquisition Time (min)

Kt qu khong tuyn tnhA e a ip id - 5 Le ls, 5 Le ls U d 5 Po t 5 Po t U d 0 Q s ctmr ve ve se , in s, in s se , C R sp n s e o se x0 5 1 0 .9 0 .8 0 .7 0 .6 0 .5 0 .4 0 .3 0 .2 0 .1 0 0 2 4 6 8 1 0 1 2 1 4 1 6 1 8 2 0

y= 6 9 8 7*x - 4 1 1 3 4 2 .5 1 5 .0 7 R 2= .9 8 5 0 ^ 0 9308

C n e t a io ( g l) o c n r t n n /m

ng chun 5 mc nng Acetamiprid

Kt qu sc k v ph ti LOD = 0,1 ng/ml+ MRM (223.0 -> 126.0) 27050806.d Abundance x10 2 1.2 1.1 1 0.9 0.8 0.7 0.6 0.5 0.4 0.3 0.2 0.1 0 -0.1 5 5.5 6 6.5 Acquisition Time (min) 223 -> 126.0 , 126.0 Relative Abundance (%) x10 4 3.2 3 2.8 2.6 2.4 2.2 2 1.8 1.6 1.4 1.2 1 0.8 0.6 0.4 0.2 0 -0.2 -0.4 5 5.5 6 6.5 Acquisition Time (min) Ratio= 100.0 + MRM (5.712-6.007 min, 43 scans) 2 Abundance x10 1 4.25 4 3.75 3.5 3.25 3 2.75 2.5 2.25 2 1.75 1.5 1.25 1 0.75 0.5 0.25 0

5.822 Acetam iprid

126.0

90.1100 150 200 Mass-to-Charge (m/z)

Kt qu lp li thit b Tng quan gia nng chun, din tch pic v t l S/N

Kt qu ti LOQ=0,006 mg/kg

Kt qu thu hi trung bnh v lp li phng php1. Mu trng( blank) thm chun cc mc nng khc nhau. 2. Phn tch lp li 5 ln ti mi nng .

Hiu sut v CV ti cc mc nng

Kt lun1. trin khai thnh cng phng php phn tch Acetamiprid trn thit b Agilent 6410-Triple. 2. Phng php xy dng cho nhy tt (LOQ = 0.006 mg/kg) chnh xc cao ( thu hi 105-120%) lp li tt ( CV< 10%).

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