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TO DOWNLOAD A COPY OF THIS POSTER, VISIT WWW.WATERS.COM/POSTERS ©2017 Waters Corporation MKT17195 QuEChERS ১峼ఒ峁峉ჼর峘嵆崌崛崰崕崟嵛峘 UPLC-MS/MS 峑峘 żম ઌ৶ 1) , Young Michael 2) , Tran Kim 2) , Shah Dimple 2) 1) ম崎崑嵤崧嵤崢ઙভ, 2) Waters Corporation INTRODUCTION ফ৫岿島峉 QuEChERS ১峼৷岮峉ჼর峘嵆崌崛崰崕崟嵛ীෲ 1) 峙岝ઽ૨峙ଐ峑岬峵岶岝ಖଲચ岶ী峑岬峵峉峫岝ৈ২峔ਫ਼ল ஓ峼ਏ峒峁峉岞ম১峑峙岝QuEChERS ১峘ಖଲ峘ী峕ৗૠ峘ಕৼ 嵇崳崓嵑嵈 Oasis PRiME HLB 峼৷岮峐岝ઽ૨峒ಖଲચ峼ఒ峁岝峲峴 岮২峘ਫ਼লஓ峕৷峑岷峵૪৶১峼ਫ਼ୈ峁峉岞 1 峕ਏ峔嵆崌崛崰崕崟嵛峘ଡୗ峼峁峉岞 1. ਏ峔嵆崌崛崰崕崟嵛峘ଡୗ METHODS SAMPLE PREPARATION QuEChERS ল ৵ 5 g 峼 50 mL 峘೫ଵ峕ো島ق崡崹崌崗મ峘峙岝岽岽峑ใ ੴ෯২峘崡崹崌崗ఏ峼ਸ岲峉ك岝10 mL 峘峒岝10 mL 峘 10:90 崖崊崣崰崳崰嵒嵓峼ਸ岲峐岝1 ৎঽஷ峒岰ਃ峕岵岻峉岞 QuEChERS ৷峘ව峼ਸ岲قWaters DisQuE 崹崎崩 ଲષಀ 186006813:1 g 崗崐嵛ਕ崲崰嵒崎嵈ਮ岝0.5 g 崗崐嵛ಞ崲 崰嵒崎嵈崣崡崕ਮ岝1 g ව৲崲崰嵒崎嵈岝4 g ૮ᆼ崲崰嵒崎嵈ك岝 峑 1 ীᒘ岝৺ 2200 rcf 峕峐 5 ী೫ী峕岵岻峉岞 dSPE ಖଲ ল峑੭峳島峉ಽ峘崊崣崰崳崰嵒嵓ಽ 5 mL 峼岝QuEChERS ৷峘ව قWaters DisQuE 崹崎崩 ଲષಀ 186008080:750 mg ૮ᆼ 嵆崘崵崟崎嵈岝150 mg C18岝150 mg 崊嵓嵇崲-N岝250 mg PSAك岶 ো峍峉 15 mL 峘೫ଵ峕峁岝峑 1 ীᒘ岝৺ 2200 rcf 峕峐 5 ী೫ী峕岵岻峉岞100 ȝL 峘峼 1.0 mL 峘ৼ A 峑ൌ 峁岝UPLC-MS/MS ীෲ峕峁峉岞 UPLC-MS/MS ীෲ UPLC ੯ LC ಎ ؟ACQUITY UPLC H-Class 崓嵑嵈 ؟ACQUITY UPLC BEH C18, 1.7 ȝm, 2.1 x 100 mm ৼ ؟A ؟0.1%崖 B ؟0.1%崖崊崣崰崳崰嵒嵓 ো ؟10 ȝL 崓嵑嵈ആ২ ؟40٦ 崳嵤崱嵓 ؟90%嵉崧崶嵤嵓 崝嵛崿嵓嵆崵嵤崠嵋崹嵤崠 ؟50%嵉崧崶嵤嵓 崟嵤嵓崎崑崫崟嵍 ؟10%嵉崧崶嵤嵓 崘嵑崠崐嵛崰 ؟MS ੯ ସীෲ ؟Xevo TQ-S micro 崌崒嵛৲嵊嵤崱؟嵅崠崮崋崾قchloramphenicol 峘峩崵崔崮崋崾 ك崌崒嵛౺ആ২ ؟150٦ ᄘ崔崡ആ২ ؟500٦ ᄘ崔崡 ؟1000 L/Hr 崛嵤嵛崔崡 ؟30 L/Hr 崯嵤崧ଵ৶ ؟MassLynx v4.1 RESULTS 2. 崰崎嵊嵕崛崟র峕ৈ෯২崡崹崌崗峁峉嵆崌崛崰崕崟嵛峘 LC-MS/MS 崗嵕嵆崰崘嵑嵈 1. MRM 崰嵑嵛崠崫崟嵏嵛岝ಎ崹嵑嵉嵤崧嵤岝৳ৎ CONCLUSION x ჼ峘 QuEChERS ল峼 dSPE 峕峲峴ಖଲ峁岝1:10 峕ൌ 峃峵峒岝ৈ২峔ਫ਼লஓ岶ਏ峑岬峍峉 x Oasis PRiME HLB 峕峲峵ಖଲ峙岝࿉૩ਛী峑岬峵ସ岴峲峝嵒 嵛ସ峼প峕ு峁岝LC-MS/MS 峕峲峵嵆崌崛崰崕崟嵛峘ผী ෲ峼২峘岮ਫ਼লஓ峑峬૭ચ峕峁峉 BETTER CLEANUP? ಖଲ峕 dSPE 峼৷岮峐岮峉峒岽峷岝Oasis PRiME HLB 嵇崳崓嵑嵈峼৻峹 峴峕৷岮峉১峑ਫ਼ୈ峼ষ峍峉岞মಖଲ১峙岝QuEChERS ল岵峳 ટ峕ସ峒嵒嵛ସ峼ு峁峉岞岽峘ટ岝ਈીಖଲ峼崐崸嵅嵔嵤 崰岝ગ峁峉岝dSPE 峘১峒ຎ峃峵峒岝ଋ᪗岶峁峉ق 4 සك岞嵒嵛ସ峕ঢ়峁峐峬峳岵峔ு岶崗嵕嵆崰崘嵑嵈峲峴ஜ峒峔峍峉 ق 5 සك岞 5. Oasis PRiME HLB 嵇崳崓嵑嵈峘ಖଲ峕峲峴岝崰崎嵊嵕崛崟峘 QuEChERS ল岵峳岝95%ਰ峘嵒嵛ସقlecithinsك峼ு峁 峉峘 LC-MS/MS 崗嵕嵆崰崘嵑嵈 Oasis PRiME HLB 嵇崳崓嵑嵈 3 cc/60 mg 峕峲峵ಖଲ 嵣QuEChERS ল 1 mL 峼峴岝300 ȝL 峘峼ਸ岲峵 嵣0.65 mL 峘ൌলقল 0.5 mL ৼਊك峼崸崕嵍嵤嵈嵆崳嵃嵤 嵓崱ق৺ 1 psiك峼৷岮峐岝嵇崳崓嵑嵈峕ಞ峴岿峅峉 嵣0.2 mL 峘 80%崊崣崰崳崰嵒嵓峼嵇崳崓嵑嵈峕峁岝ಞ峴ী峒 峹峅峉 嵣ಞ峴ী峕 1 mL 峘崊崣崰崳崰嵒嵓峼ਸ岲岝崐崸嵅嵔嵤崰峼ষ峍峉 嵣ᄚಞਞ峑ಕ峁峉 嵣200 ȝL 峘ৼ峑ગ峁峉 Aflatoxin B1 Deoxynivalenol Zearalenone Fumonisin B2 Ochratoxin A Time (min) Flow (mL/min) %A %B Curve Initial 0.400 90 10 initial 3.00 0.400 90 10 6 10.00 0.400 30 70 6 10.10 0.400 10 90 6 12.00 0.400 10 90 6 12.10 0.400 90 10 6 15.00 0.400 90 10 6 Time 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 2.00 4.00 6.00 8.00 % 0 100 7.54 7.24 7.22 6.90 6.88 6.35 7.22 7.32 8.27 1.74 7.53 Citrinin Aflatoxin G2 Aflatoxin G1 Aflatoxin B1 Aflatoxin B2 Deoxynivalenol Fumonisin B1 Time 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 2.00 4.00 6.00 8.00 10.00 % 0 100 8.32 8.01 8.12 7.93 8.23 1.07 1.12 9.44 8.63 9.14 9.40 8.80 9.73 Zearalenone T 2 Toxin Ochratoxin B Ochratoxin A Nivalenol HT2 Toxin Fumonision B2 Compound MRM Cone (V) Collision (eV) Spike Level (low,high) (μg/kg) RT Aflatoxin B1 313.00> 241.10 5 40 1, 10 7.54 313.00> 285.20 5 28 Aflatoxin B2 315.00> 259.10 20 33 1, 10 7.24 315.00> 287.10 20 30 Aflatoxin G1 329.00> 311.10 20 20 1, 10 7.22 329.00> 243.10 20 35 Aflatoxin G2 331.00> 245.10 20 25 1, 10 6.89 331.00> 313.10 20 28 Citrinin 251.10> 233.20 20 20 25, 250 8.27 251.10> 205.20 20 28 Deoxynivalenol 297.10> 231.10 15 18 125, 1250 1.74 297.10> 249.10 15 18 Fumonisin B1 722.50> 334.20 30 40 125, 1250 7.53 722.50> 352.20 30 35 Fumonisin B2 706.50> 336.20 35 40 125, 1250 8.33 706.50> 318.20 35 40 HT2 toxin 442.20> 263.20 25 12 25, 250 8.12 425.10> 245.20 45 12 Nivalenol 313.10> 175.10 15 13 125, 1250 1.07 313.10> 247.20 15 10 Ochratoxin A 404.10> 239.10 20 25 2.5, 25 9.44 404.10> 358.10 20 16 Ochratoxin B 370.10> 205.20 20 24 2.5, 25 8.63 370.10> 187.10 20 25 T 2 Toxin 484.20> 305.20 25 9 25, 250 9.13 484.20> 245.20 25 9 Zearalenone 319.10> 283.30 15 13 25, 250 9.40 319.10> 187.20 15 15 Maize Rice Wheat % Recovery (% RSD) % Recovery (% RSD) % Recovery (% RSD) low high low high low high Alfatoxin B1 95 (6) 104 (8) 116 (12) 120 (10) 114 (8) 95 (5) Aflatoxin B2 103 (11) 109 (8) 119 (7) 115 (6) 109 (12) 87 (9) Alfatoxin G1 96 (9) 106 (8) 109 (7) 114 (9) 133 (13) 98 (4) Aflatoxin G2 89 (12) 109 (6) 99 (12) 118 (6) 109 (13) 98 (28) Citrinin 79 (15) 77 (9) 83 (5) 84(2) 112(17) 110(18) Deoxynivalenol 103 (11) 106 (5) 99 (4) 90 (3) 100 (10) 97 (3) Fumonisin B1 INC 85 (14) 97 (4) 72 (6) 97 (8) 82 (9) Fumonisin B2 85 (20) 89 (12) 108 (3) 86 (4) 107 (6) 101 (11) HT2 Toxin BLOQ 158 (4) 101 (11) 112 (3) 115 (16) 89 (12) Nivalenol BLOQ 73 (4) BLOQ 71 (3) 55 (14) 63 (6) Ochratoxin A 103 (3) 100 (2) 107 (7) 103 (1) 113 (2) 117 (6) Ochratoxin B 104 (4) 101 (2) 110 (3) 103 (2) INC 115 (26) T2 Toxin 57 (9) 40 (8) 97 (5) 99 (3) 116 (12) 121 (18) Zearalenone 115 (21) 88 (16) 109 (21) 103 (12) 96 (21) 115 (10) 2.ਸઽୡ峘ટقBLOQ ؟கਰ岝INC ؟崡崹崌崗 ෯২峘 10%ਰ峘ใோ崾嵑嵛崗 ك 3.৵岴峲峝崰崎嵊嵕崛崟র峘嵆崌崛崰崕崟嵛峘ใோ崾嵑嵛崗 DISCUSSION x ফ৫岿島峉 QuEChERS ১峙岝৵岝崰崎嵊嵕崛崟岝৪峕 ৌ峁峐嵆崌崛崰崕崟嵛峘ผল峕ટ峑岬峍峉 x dSPE 峕峲峵ಖଲ峙岝ઽ૨峙ౄী峑岬峵岶岝ಖଲચ岶ী峑岬 峵峉峫岝ৈ২峔ਫ਼লஓ峼ઞ৷峁峔岮峒ৌ峃峵岽峒岶峑岷峔岵峍峉 4. ం峘ઌ峙岝崰崎嵊嵕崛崟峘 QuEChERSল 峼Oasis PRiME HLB嵇崳崓嵑嵈峒dSPE峑ಖଲ峁峉ટ峘ຎ岞క峘ઌ峙岝ಖ ଲ0.5 mL峼崐崸嵅嵔嵤崰岝0.2 mL峕ગ峁峉峘ଋ᪗峘ୀ岮岞 Oasis PRiME HLB dSPE Oasis PRiME HLB dSPE Time 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 % 0 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 % 0 myco09082034a 1: MRM of 12 Channels ES+ TIC (phospholipid) 1.21e7 10.34 10.15 10.95 11.35 myco09082033a 1: MRM of 12 Channels ES+ TIC (phospholipid) 1.21e7 dSPE ಖଲ Oasis PRiME HLB ಖଲ References 1. U. Koesukwiwa et al., "Evaluation of a modified QuEChERS method for analysis of mycotoxins in rice", Food Chemistry, 153 (2014) 44–51
Transcript of Ø - Waters Corporation · 2017-10-26 · MRM]0]Q][] ]+] ]O][\ ¼]9]Q]I]d]']d\ ó E Î Ñ C C ... T...
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QuEChERSUPLC-MS/MS
1) , Young Michael 2), Tran Kim 2), Shah Dimple 2) 1) , 2)Waters Corporation
INTRODUCTIONQuEChERS 1)
QuEChERSOasis PRiME HLB
1
1.
METHODSSAMPLE PREPARATION
QuEChERS
5 g 50 mL10 mL 10 mL 10:90
1
QuEChERS Waters DisQuE186006813:1 g 0.5 g
1 g 4 g 1 2200 rcf 5
dSPE
5 mL QuEChERSWaters DisQuE 186008080:750 mg
150 mg C18 150 mg -N 250 mg PSA15 mL 1 2200 rcf 5
100 L 1.0 mL AUPLC-MS/MS
UPLC-MS/MS
UPLCLC ACQUITY UPLC H-Class
ACQUITY UPLC BEH C18, 1.7 m, 2.1 x 100 mm
A 0.1%B 0.1%
10 L 40
90%50%
10%
MSXevo TQ-S micro
chloramphenicol150
5001000 L/Hr
30 L/Hr MassLynx v4.1
RESULTS
2. LC-MS/MS
1. MRM
CONCLUSIONQuEChERS dSPE 1:10
Oasis PRiME HLBLC-MS/MS
BETTER CLEANUP?
dSPE Oasis PRiME HLBQuEChERS
dSPE 4
5
5. Oasis PRiME HLBQuEChERS 95% lecithins
LC-MS/MS
Oasis PRiME HLB 3 cc/60 mg
QuEChERS 1 mL 300 L0.65 mL 0.5 mL
1 psi
0.2 mL 80%
1 mL
200 L
Aflatoxin B1 DeoxynivalenolZearalenone
Fumonisin B2Ochratoxin A
Time(min)
Flow(mL/min) %A %B Curve
Initial 0.400 90 10 initial3.00 0.400 90 10 610.00 0.400 30 70 610.10 0.400 10 90 612.00 0.400 10 90 612.10 0.400 90 10 615.00 0.400 90 10 6
Time2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100
2.00 4.00 6.00 8.00
%
0
100 7.54
7.24
7.22
6.90
6.88
6.357.22
7.32
8.27
1.74
7.53
Citrinin
Aflatoxin G2
Aflatoxin G1
Aflatoxin B1
Aflatoxin B2
Deoxynivalenol
Fumonisin B1Time
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100
2.00 4.00 6.00 8.00 10.00
%
0
100 8.32
8.01
8.12
7.93 8.23
1.07
1.12
9.44
8.63
9.14
9.40
8.80 9.73Zearalenone
T 2 Toxin
Ochratoxin B
Ochratoxin A
Nivalenol
HT2 Toxin
Fumonision B2
Compound MRM Cone (V)Collision(eV)
Spike Level(low,high)(μg/kg) RT
Aflatoxin B1 313.00> 241.10 5 40 1, 10 7.54313.00> 285.20 5 28
Aflatoxin B2 315.00> 259.10 20 33 1, 10 7.24315.00> 287.10 20 30
Aflatoxin G1 329.00> 311.10 20 20 1, 10 7.22329.00> 243.10 20 35
Aflatoxin G2 331.00> 245.10 20 25 1, 10 6.89331.00> 313.10 20 28
Citrinin 251.10> 233.20 20 20 25, 250 8.27251.10> 205.20 20 28
Deoxynivalenol 297.10> 231.10 15 18 125, 1250 1.74297.10> 249.10 15 18
Fumonisin B1 722.50> 334.20 30 40 125, 1250 7.53722.50> 352.20 30 35
Fumonisin B2 706.50> 336.20 35 40 125, 1250 8.33706.50> 318.20 35 40
HT2 toxin 442.20> 263.20 25 12 25, 250 8.12425.10> 245.20 45 12
Nivalenol 313.10> 175.10 15 13 125, 1250 1.07313.10> 247.20 15 10
Ochratoxin A 404.10> 239.10 20 25 2.5, 25 9.44404.10> 358.10 20 16
Ochratoxin B 370.10> 205.20 20 24 2.5, 25 8.63370.10> 187.10 20 25
T2 Toxin 484.20> 305.20 25 9 25, 250 9.13484.20> 245.20 25 9
Zearalenone 319.10> 283.30 15 13 25, 250 9.40319.10> 187.20 15 15
Maize Rice Wheat%Recovery (% RSD) %Recovery (% RSD) %Recovery (% RSD)
low high low high low high
Alfatoxin B1 95 (6) 104 (8) 116 (12) 120 (10) 114 (8) 95 (5)
Aflatoxin B2 103 (11) 109 (8) 119 (7) 115 (6) 109 (12) 87 (9)
Alfatoxin G1 96 (9) 106 (8) 109 (7) 114 (9) 133 (13) 98 (4)
Aflatoxin G2 89 (12) 109 (6) 99 (12) 118 (6) 109 (13) 98 (28)
Citrinin 79 (15) 77 (9) 83 (5) 84(2) 112(17) 110(18)
Deoxynivalenol 103 (11) 106 (5) 99 (4) 90 (3) 100 (10) 97 (3)
Fumonisin B1 INC 85 (14) 97 (4) 72 (6) 97 (8) 82 (9)
Fumonisin B2 85 (20) 89 (12) 108 (3) 86 (4) 107 (6) 101 (11)
HT2 Toxin BLOQ 158 (4) 101 (11) 112 (3) 115 (16) 89 (12)
Nivalenol BLOQ 73 (4) BLOQ 71 (3) 55 (14) 63 (6)
Ochratoxin A 103 (3) 100 (2) 107 (7) 103 (1) 113 (2) 117 (6)
Ochratoxin B 104 (4) 101 (2) 110 (3) 103 (2) INC 115 (26)
T2 Toxin 57 (9) 40 (8) 97 (5) 99 (3) 116 (12) 121 (18)
Zearalenone 115 (21) 88 (16) 109 (21) 103 (12) 96 (21) 115 (10)
2. BLOQ INC10%
3.
DISCUSSIONQuEChERS
dSPE
4. QuEChERS Oasis PRiME HLB dSPE
0.5 mL 0.2 mL
Oasis PRiME HLB dSPE Oasis PRiME
HLB dSPE
Time4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00
%
0
4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00
%
0
myco09082034a 1: MRM of 12 Channels ES+ TIC (phospholipid)
1.21e710.34
10.15
10.95
11.35
myco09082033a 1: MRM of 12 Channels ES+ TIC (phospholipid)
1.21e7
dSPE
Oasis PRiME HLB
References 1. U. Koesukwiwa et al., "Evaluation of a modified QuEChERS
method for analysis of mycotoxins in rice", Food Chemistry, 153 (2014) 44–51
