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LC/MS電離技術及在藥品雜質和降解產物的發(fā)現(xiàn)及分析方法Speaker
Name：趙貴平
Speaker
Title:
ProductManagerApplied
Markets
:
AB
SCIEX
Marketing
team
China不同電離源的適用范圍2March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND光致離子化化學離子化電噴霧離子化電噴霧離子化(ESI)–顯示正電離模式氣簾氣(CUR)溶劑蒸發(fā)庫倫排拆電離噴務電壓霧化氣(GS1)液相流動相形成帶電小液滴錐孔(DP)質量分析器真空大氣壓條件加熱器及輔助霧化氣(GS2)1.
2.
3.3March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND形成帶電液滴液滴蒸發(fā)，液滴里的場強增加離子從液滴中迸發(fā)出來，在接口處聚焦帶電溶劑分子與分析物分子進行電荷交換放電針(NC)錐孔(DP)質量分析器氣簾氣(CUR)真空大氣壓條件液相流動相X=溶劑分子M=目標分子霧化加熱器(TEM)4March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND霧化氣(GS1)1.
2.溶劑分子離子化3.形成帶電離子大氣壓化學離子化(APCI)離子源在源內使N2或O2離子化N2或O2將電荷傳給溶劑蒸汽蒸發(fā)的帶電溶劑將電荷傳給化合物大氣壓光離子化(APPI)APPI中倆個離子化機制:電荷在非極性化合物間傳遞(上面所示)極性化合物溶劑傳遞..5March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND.離子源優(yōu)缺點6March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDESI優(yōu)點
適合大范圍的化合物-大小分子和極性化合物熱不穩(wěn)定性和揮發(fā)性化合物最溫和的分子碎裂方式可分析大分子量（多電荷）化合物高靈敏度缺點離子抑制：靈敏度受流動相組成的影響APCI
&
APPI優(yōu)點低極性化合物寬動態(tài)范圍(4-5
個數(shù)量級）質量敏感（依賴流速）可耐受高緩沖液濃度缺點要求化合物熱穩(wěn)定(最高130-150°C)揮發(fā)性需要助劑(APPI
)藥品雜質和降解產物的發(fā)現(xiàn)及分析方法7March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND藥品雜質和降解產物在藥劑學中的重要性藥品雜質和降解產物的發(fā)現(xiàn)及分析方法與技術藥品雜質和降解產物在藥劑學中的重要性8March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND藥劑學–“生產可行性和可控性”藥物的早期發(fā)現(xiàn)原型藥物原型配方可溶解性穩(wěn)定性評價ICH要求的穩(wěn)定性試驗(藥物和成品)ICH
要求的雜質分析藥物開發(fā)原型配方的毒性研究詳細的物理化學特性雜質分析鑒定藥物篩選結構特征早期雜質鑒定和分析9March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND藥物配方研制過程添加物藥品藥品的穩(wěn)定性輔料兼容性配方開發(fā)包裝選擇活性藥物成分包裝材料成藥10March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND貯藏條件活性成分的穩(wěn)定性產生過程中的雜質潛在雜質來源11March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND活性藥物成分/輔料的雜質:合成前體合成共生體溶劑殘留催化劑分解物其它雜質藥品的雜質:降解產物提取物溶劑殘留未知物ICH
Q3:12March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND雜質含量必須少于申報低限(人用藥品注冊技術要求國際協(xié)調會)藥物活性成分成藥<=2g/day>
2g/day<=1g/day>1g/day報低限0.05%0.03%0.10%0.05%鑒定低限0.10%0.05%1%1%定量低限0.15%0.05%1%1%降解物的獨特性13March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDICH
Q2A:對于在藥品產生過程中,藥物本體和活性成分的激化反應研究（如:產品的酸堿水解,熱降解，光解，氧化)應提供具有獨特性的檢測和雜質分析方法。目的合成足夠多典型穩(wěn)定性的降解產物以便于分析鑒定避免二次降解–通過化驗評估,降解范圍控制在5-20%以內–觀察純度和質量平衡藥品雜質和降解產物的發(fā)現(xiàn)及分析方法與技術14March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDLC-UV三重四極桿質譜技術–
用MRM,
母離子,中性丟失掃描鑒定未知雜質離子阱質譜技術高分辨質譜技術LC-NMRQTRAP質譜技術--三重四極桿線性離子阱復合技術其它技術15March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND藥品雜質和降解產物的發(fā)現(xiàn)及分析方法與技術工作量質譜技術的選擇?90%10-5%<5%串聯(lián)四極桿質譜3-D以及線性離子阱質TOF,FTQTRAP技術16March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND不同質譜技術的應用串聯(lián)四極桿中的多反應監(jiān)察用定量分析和ADMET的評價母離子掃描,中性丟失掃描的未知物鑒定離子阱和MS3用于未知物鑒定的代謝物鑒定以極結構分析高分辨質譜的結構鑒定三重四極桿串聯(lián)質譜線性離子阱質譜4000
Q
TRAP?Q
TRAP
系統(tǒng):串聯(lián)四極桿線性離子阱復合質譜技術3200
Q
TRAP?QTRAP
550017March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDAB
QTRAP串聯(lián)四極桿線性離子阱質譜18March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND六種增強型掃描方式增強分辨掃描(ER)增強子離子掃描(EPI)MS/MS/MS
(MS3)增強全掃描(EMS)增強多電荷掃描(EMC)時間延遲碎片掃描(TDF)全掃描子離子掃描功能母離子掃描功能多反應監(jiān)檢掃描MRM中性丟失掃描功能選擇離子掃描SIR這兩種質譜技術用軟件的掃描聯(lián)動功能IDA,可同時采集質譜數(shù)據(jù)Q
TRAP
液質聯(lián)用系統(tǒng)-<1ms
切換從QQQ
到QqLIT-MS/MS
子離子掃描靈敏度
>500x
比QQQ19March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDQ3Radial
TrappingRadial
TrappingAxialTrapping20March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDRadial
TrappingRadial
TrappingAxialTrappingAxialTrappingAux
RfIons
“Jump”
the
Exit
Barriervia.
Fringing
Fields
and
thewell
created
in
the
Grid
EXBExit
Lenswith
Grid21March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND三重四極桿串聯(lián)質譜多反應離子監(jiān)測MRM子離子掃描母離子掃描中性丟失掃描全掃描SIMQtrap：解決同時定量定性問題線性離子阱質譜增強子離子掃描(EPI)MS3增強全掃描(EMS)增強多電荷掃描(EMC)增強高分辨掃描時間延遲碎裂掃描(TDF)復合掃描方式MRM-EPI（子離子掃描）MRM-MS3母離子掃描-EPI中性丟失掃描-EPIEMS
–EPI?……靈敏度、穩(wěn)定性、重現(xiàn)性完全一致22March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND定量和定性一次完成…MRM
Enhanced
Product
Ion(EPI)實驗Multiple
MRM’sIDA
CriteriaLevel
1EPIAdd
toExclusion
ListMRM
掃描可作為IDA預掃描:23March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND利用MRM的高選擇性和高靈敏度利用LINAC
碰撞室可檢測多種離子對(一次進樣可檢測~300
對離子對)MRM
然后觸發(fā)EPI掃描，在線采集MS/MS圖譜用于確證MRM
數(shù)據(jù)仍能用于定量IDA(Information
Dependent
Acquisition
，信息相關采集)如何利用QTRAP技術進行雜質和降解產物的鑒定24March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND優(yōu)化化合物電離參數(shù)，獲得其二級質譜碎片規(guī)律用LightSight?軟件2.0
建立分析方法EMS掃描檢測含量高的雜質和降解產物低含量的雜質和降解產物用:母離子掃描(活性成分的母離子掃描)中性丟失掃描(活性成分的中性掃描I)數(shù)據(jù)用LightSight?軟件處理25March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDQTRAP
技術鑒定雜質和降解產物活性成分的分子量MW=167鑒定在制劑溶液中熱處理藥物產品的降解產物降解產物和標樣的比較26March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND使用3200QTRAP系統(tǒng)的不同掃描方式分析雜質及降解產物實驗步驟27March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND液相方法:進樣量為10
L(濃度為10ng/
L)色譜柱:2.0
x
150
mm
3um流動相A:含5
mM乙酸胺的超純水流動相B:含5
mM
乙酸胺的乙腈用3200QTRAP系統(tǒng)的EMS,
Precursor,
NL
和MRM
掃描方法建立分析方法用LightSight軟件處理兩種樣品的數(shù)據(jù)3200QTRAP?
系統(tǒng)結合LightSight
2.0TM
軟件處理數(shù)據(jù)28March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDEMS掃描發(fā)現(xiàn)m/z
168.1(活性成分)確定母離子的保留時間以便確定其二級質譜圖29March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDEMS掃描發(fā)現(xiàn)m/z162(比活性成分減小6個質量數(shù))30March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDEMS掃描發(fā)現(xiàn)m/z
394(比活性成分增加226)31March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDm/z
394的二級質譜圖32March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND中性丟失18掃描發(fā)現(xiàn)m/z272三上峰(比活性成分增加104)33March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND母離子掃描135,發(fā)現(xiàn)m/z17034March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDm/zGain/lossRT
(min)EMSPrec107Prec121NL18MRM154-145.36180+125.65170+25.72180+126.03165-36.08394+2266.33162-46.67272+1048.36272+1049.14272+1049.71280+1128.94280+11210.9435March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND發(fā)現(xiàn)了12個潛在的降減產物及雜質總結用4000QTRAP系統(tǒng)分析奧美拉唑的雜質及降解產物36March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND樣品處理酸降減:10N鹽酸加入奧美拉唑(濃度為0.2mg/ml)溶液中,此溶液用硼酸鈉溶液(10mM)緩沖pH9.2;五分鐘后,用10N氫氧化鈉溶液中和.堿降減:10N氫氧化鈉加入奧美拉唑(濃度為0.2mg/mL)溶液中,五分鐘后,用10N的鹽酸溶液中和溶液.實驗條件37March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND質譜儀AB
SCIEX
4000QTRAP系統(tǒng)流動相A:乙腈,流動相B:含1.5
mM磷酸鈉的超純水流速:0.8
mL/min.色譜柱:Zorbax
C18
4.6
x
150
mm,5um奧美拉唑的雜質及降解產物的檢測38March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND結論奧美拉唑的可能降減產物39March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND流動相中使用磷酸鹽緩沖鹽并不影響靈敏度分析樣品8小時后,磷酸鈉緩沖鹽結晶在錐孔上的情形并汪影響分析的靈敏度40March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND用ABSCIEX公司的3200QTRAP系統(tǒng)檢測抗倒酯的雜質用QTRAP技術中的增強全掃描（EMS）一次進樣，可檢測出9個雜質41March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND液相條件42March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND島津二元高壓液相系統(tǒng)色譜柱:C18
2.1X150mm流動相:A:
含0.1%甲酸的超純水B:
含0.1%甲酸的乙腈流速:300
uL/min進樣體積:10uL樣品濃度:1mg/mLESI負離子EMS掃描:抗倒酯的保留時間為15.7min;
還有其它9個雜質化合物抗倒酯Scale
change43March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND??ESI正離子EMS掃描:抗倒酯保留時間為15.7
min;
還有9個雜質抗倒酯Scale
changeMarch,
2009,
Beijing,
China
?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
Owners
ABOVE
&
BEYON44DEMS負離子掃描:抗倒酯的質譜圖RT=15.7
min(MW=252;
neg
251)45March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDEMS正離子掃描:抗倒酯質譜圖RT=15.7
min(MW=252;
pos
253)46March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDESM負離子:抗倒酯的雜質質譜圖RT=7.7
min47March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDEMS正離子掃描:抗倒酯的雜質質譜圖RT=7.7
min48March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND只有正離子掃描才有信號的抗倒酯雜質RT=16.7
min49March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND樣品中植物生長因子的分析Speaker
Name：趙貴平
Speaker
Title:
Product
ManagerApplied
Markets
:
PSM
Marketing
team
China吲哚乙酸的結構51March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDLC/MS/MS分析方法52March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND色譜方法：液相色譜儀:島津２０ＡＤ二元高壓系統(tǒng)色譜柱:Waters
Altantis
C18
2.1*150mm
5um色譜柱溫度：３０度進樣量：5ul流動相:
A:水,B:乙腈,
梯度冼脫梯度表:Time(min)Flow
rate(ul/min)A%B%0200901010200109015200109015.12001090202001090LC/MS/MS分析方法質譜條件：質譜儀：美國應用生物系統(tǒng)公司API
3200QTRAP系統(tǒng)電離方式：ESI+采集方式：MRM-IDA-EPI(同時定量定性分析）儀器參數(shù)：Curtain
gas=10,
Collision
gas=
5,
IonsprayVoltage=5500,
Temperature=600,
Ion
Sourcegas1=60,
Ion
Source
gas2=50,
InterfaceHeater=on, Entaance
Potential=10,
Collision
cellexit
Potential=3.53200
Q
TRAP?LC/MS/MS
System53March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND標準樣品的質譜信息標準樣品溶液通過直接進樣，發(fā)現(xiàn)除吲哚乙酸分子離子（m/z176）外，還發(fā)現(xiàn)一些其它化合物的信息，再通過子離子掃描方式，確定了相應的子母離子對，從而確定了下面相應的MRM。54March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND化合物名稱Q1Q3DPCE未知物130.184.17023吲哚乙酸176.1130.211025未知物190.1130.16025未知物220.1150.112017未知物268.1164.19030未知物268.1162.19025未知物268.1206.19025標準樣品的總離子流圖（MRM）TIC
o
f
+
MRM
(7
pa
irs):
E
xp
1,
from
Sam
pl
e
1
0
(jin_
std_
epi4
0)
of
zh
ao_
jin.wiff
(Tur
bo
Sp
ray)M
ax.
5.
6e
6
cp
s.1234567891213141
5161
718192
01
0
11Ti
me
,
m
in0
.05
.0e
51
.0e
61
.5e
62
.0e
62
.5e
63
.0e
63
.5e
64
.0e
64
.5e
65
.0e
65
.5e
612.4113.
8114.0515
.5
211.3255March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為3.5min的色譜峰（m/z130)XIC
of
+MRM
(7
p
airs):
E
xp
1
,
13
0.1/84.1
amu
from
Samp
le
8
(jin_
std_
epi5
0)
of
zh
ao_
jin.wiff
(Turbo
Spray),
Smoothed
,
SmoothedMax.
1.1e
4
cp
s.12345679101112131415168Time
,
min1000.00500.000
.002000.001500.003000.002500.005500.005000.004500.004000.003500.006500.006000.007500.007000.001
.05
e41
.00
e49500.009000.008500.008000.001
.15
e41
.10
e43
.52
2.192
.03
1.502
.28
1.324.057.198
.483.360
.11
9.317.7
65.48
5.91
6
.4
24.53
5.299.78
10
.5
910.97
11.94
12.1513.20
13.4714
.2156March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND三種不同CE的EPI質譜圖(m/z130)+EPI
(130.10)
Charge
(+
0)
C
E
(25)
C
ES
(5)
FT
(250):
Exp
2,
3.277
to
3.685
min
fro...
Max.
8.2e4
cps.8.0
e4
130.26.0
e4
CE=304.0
e42.0
e4
129.150
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200m/
z,
amu+EPI:
Exp
2,
3.402
to
3.630
min
from
Sample
10
(jin_std_epi40)
of
zhao_jin.wiff
(Tu...
Max.
7566.8
cps.7567
103.0130.16000
77.0129.0
CE=404000
102.165.9
67.8
128.12000
74.9
95.050
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200m/
z,
amu+EPI
(130.10)
Charge
(+
0)
C
E
(60)
FT
(250):
Exp
2,
3.568
to
3.761
min
from
Sampl...
Max.
4006.7
cps.4000
77.03000
CE=602000
66.467.4
75.0101.91000
55.6
95.150
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200m/
z,
amu57March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為11.38min色譜峰（m/z176.1)XIC
of
+MRM
(7
pairs):
Exp
1,
176.1/130.2
amu
from
Sample
8
(jin_std_epi50)
of
zhao_jin.wiff
(Turbo
Spray)Max.7.4e5
cps.12345678111213141516171819209
10Time,
min0.07.0e56.5e56.0e55.5e55.0e54.5e54.0e53.5e53.0e52.5e52.0e51.5e51.0e55.0e47.4e5Intensity,
cps11.3812.0858March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND三種不同CE的EPI質譜圖（m/z176)+EPI
(176.10)
C
harge
(+
0)
C
E
(5)
C
ES
(50)
FT
(126.533):
Exp
2,
11.330
to
11.493
...
Max.
1.0e5
cps.1.00e5
176.2CE=305.00e4130.2103.050
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200m/z,
amu+EPI
(176.10)
C
harge
(+
0)
C
E
(40)
FT
(8.36284):
Ex
p
2,
11.256
to
11.480
min
from
...
Max.
6.3e6
cps.6.5e6
130.15.0e6
CE=40103.0129.10.050
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200m/z,
amu+EPI
(176.10)
C
harge
(+
0)
C
E
(60)
FT
(250):
E
xp
2,
11.207
to
11.451
min
from
Sam...
Max.
9.7e5
cps.103.077.0129.9
CE=605.0
e565.8
68.9
89.0
95.00.050
60
70
80
90
100
110
12
0
130
140 1
50
160
170
180
190
20
0m/
z,
a
m
u59March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為12.41min色譜峰（m/z190.1)XIC
of
+MRM
(7
pairs):
Exp
1,
190.1/130.1
amu
from
Sample
10
(jin_std_epi40)
of
zh...Max.
5.6e6
cps.12345678111213141516171819209
10Tim
e,
m
in0.05.5
e65.0
e64.5
e64.0
e63.5
e63.0
e62.5
e62.0
e61.5
e61.0
e65.0
e512.4111.3160March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND三種不同CE的EPI質譜圖(m/z190.2)+E
PI:
E
xp
2,
12.278
to
12
.804
m
in
from
Sam
ple
8
(jin_std_epi50
)
of
zhao_jin.wi
ff
(T
... M
ax.
1761.4
cps.1761
190.21500CE=301000500
130.250
60
70
80
90 10
0
110 12
0
130
140
150
16
0
1
70
180
1
90
200
2
10
220
2
30 24
0
250 26
0m/
z,
a
m
u+E
PI
(176
.10)
C
harge
(+
0)
C
E
(40
)
F
T
(250
):
E
xp
2,
12
.271
to
12
.681
m
in
from
S
am
... M
ax.
2
.5
e
5
cps.2.5
e5
129.92.0
e5
CE=401.5
e51.0
e55.0
e4
103.050
60
70
80
90
1
00
1
10
120
1
30
140
1
50
160
1
70
180
1
90
200
2
10
220
2
30
240
250
260m/
z,
a
m
u+E
PI
(176
.10)
C
harge
(+
0)
C
E
(60
)
F
T
(250
):
E
xp
2,
12
.306
to
12
.709
m
in
from
S
am
... M
ax.
4
.3
e
4
cps.103.04.0
e4
130.23.0
e4
77.0
CE=602.0
e4102.21.0
e4
65.1
69.2
75.9
89.0
95.0
128.252.160
70
80
9
0
100
110
120
130 14
0
150 16
0
170 18
0
190
200
2
10
220
2
30
240
2
50
260m/
z,
a
m
u61March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為13.05min色譜峰（m/z220.1)XIC
of
+MRM
(7
pairs):
Exp
1,
220.1/150.1amu
from
Sample
9
(jin_std_epi50)of
zh...Max.
1620.0
cps.12345678111213141516171819209
10Time,
min0200100300600160015001400130012001100100090080070013.051.315001.164005.3213.8819.639.256.931.819.73
9.9662March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為13.05min色譜峰,由于其含量很小,所以沒有EPI數(shù)據(jù).63March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為13.80min色譜峰(m/z268.1)XIC
of
+MRM
(7
pairs):
Exp
1,
268.1/162.1
amu
from
Sample
10
(jin_std_epi40)
of
zh...Max.
1.1e6
cps.12345678111213141516171819209
10Time,
min0.001.00e69.00e58.00e57.00e56.00e55.00e54.00e53.00e52.00e51.00e51.14e61.10e613.8014.0515.5364March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND三種不同CE的EPI質譜圖(m/z268.2)+E
PI
(
268
.10)
C
h
arge
(
+
0)
C
E
(
5
)
C
ES
(
5
0)
F
T
(250
)
:
Ex
p
2,
13
.734
to
13
.960
m
in
fr... M
a
x.
6.7
e4
cp
s.268.26
.0e4
CE=304
.0e42
.0e460 7
0
80
90 1
00
1
10
1
20
1
3
0 14
0
15
0
16
0
1
70
180
1
90
20
0
210
22
0
230
240
2
50
260
27
0
280
29
0
3
00m
/
z,
a
m
u+E
PI
(
268
.10)
C
h
arge
(
+
0)
C
E
(
4
0
)
F
T
(54.9
638):
Ex
p
2,
13.7
43
to
13.9
09
m
i
n
from
... M
a
x.
1.2
e6
cp
s.1
.19e6
164.21
.00e6
107.0CE=405
.00e5
136.267.9
79.0
105.0
150.2
162.2
206.250 6
0
70
80
90
100
1
10
120
13
0
1
40
150
1
60 17
0
180
1
90
2
0
0
2
1
0
22
0
230
2
40
25
0
260
27
0
2
80
290
300m
/
z,
a
m
u+E
PI
(
268
.10)
C
h
arge
(
+
0)
C
E
(
6
0
)
F
T
(170.973):
Ex
p
2,
13.7
70
to
13.9
28
m
i
n
from
... M
a
x.
2.8
e5
cp
s.2
.8e5
77.0
81.02
.0e5
65.8
CE=60108.069.51
.0e5
51.7
91.0
95.0
105.0
135.9
164.250 6
0
70 8
0
90 10
0
110
12
0
130
140
1
50
160
1
70
18
0
190
20
0
210
220
2
30
240
2
5
0
260
27
0
280
29
0
3
00m
/
z,
a
m
u65March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDMRM分別為268/164和268/206的色譜圖XIC
of
+MRM
(7
pairs):
Exp
1,
268.1/164.1
amu
from
Sample
10
(jin_std_epi40)
of
zh...
Max.
8.7e5
cps.8.7
e5
14.058.0
e5
13.817.0
e56.0
e5
15.525.0
e54.0
e53.0
e52.0
e51.0
e50.0
13.421
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19T
im
e,
minXIC
of
+MRM
(7
pairs):
Exp
1,
268.1/206.1
amu
from
Sample
10
(jin_std_epi40)
of
zh...
Max.
5.5e5
cps.5.5
e5
13.815.0
e54.0
e53.0
e5
14.052.0
e5
15.531.0
e50.01
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19T
im
e,
min66March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為14.06min的三種不同CE的EPI質譜圖+EPI
(268.10)
C
harge
(+
0)
C
E
(5)
C
ES
(50)
FT
(250):
Ex
p
2,
13.992
to
14.122
m
in
fr...
Max.
4.9e4
cps.268.24.0
e4
CE=302.0
e4164.2
206.20.050
60
70
80
90
100
110
120
130
140
150
160
170
180
190
200
210
220
230
240
250
260
270
280
290
300m/
z,
am
u+EPI
(268.10)
C
harge
(+
0)
C
E
(40)
FT
(24.6709):
Ex
p
2,
14.011
to
14.139
min
from
...
Max.
2.1e6
cps.164.22.0
e61.5
e6
CE=401.0
e6135.95.0
e5
108.0
147.150
60
70
80
90
100
1
10
120
1
30
140
150
160
170
180
190
200
210
220
230
240
250
260
270
280
290
300m/
z,
am
u+EPI
(268.10)
C
harge
(+
0)
C
E
(60)
FT
(250):
Exp
2,
13.992
to
14.198
min
from
Sam...
Max.
1.3e5
cps.1.28e5
91.0
108.01.00e5
136.0
164.2
CE=6093.05.00e4
65.2
68.2
77.0
80.0
147.2103.0
122.057.4
74.3
89.2
118.050
60
70
80
90
100
1
10
120
1
30
140
150
160
170
180
190
200
210
220
230
240
250
260
270
280
290
300m/
z,
am
u67March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND保留時間為15.56min的三種不同CE的EPI質譜圖+E
PI:
E
xp
2,
15.401
to
15.687
m
in
from
Sam
ple
8
(jin_std_epi50)
of
zhao_jin.wiff
(Tu... M
ax.
1.4e4
cps.1.4
e4
268.21.0
e4
CE=305000.
05
0
60
70
80
90 10
0
11
0
12
0
13
0
14
0
15
0
16
0
1
7
0
1
8
0
1
9
0
2
0
0
2
1
0
2
2
0
2
3
0
2
40
2
50
2
60
2
70
2
80
2
90
3
00m/
z,
a
m
u+E
PI
(268.10)
C
harge
(+
0)
C
E
(40)
FT
(50.8035):
Ex
p
2,
15.471
to
15.596
m
in
from
... M
ax.
1.9e6
cps.1.9
e6
164.21.5
e6
CE=401.0
e65.0
e5
135.9108.2
147.250
60 7
0
80 9
0 100
1
10
1
20
1
30
1
40
1
50
1
60
1
70
180
1
90
200
2
10
220
2
30
2
40
2
50
2
60
2
7
0
280
2
90
30
0m/
z,
a
m
u+E
PI
(268.10)
C
harge
(+
0)
C
E
(60)
FT
(63.3086):
Ex
p
2,
15.525
to
15.643
m
in
from
... M
ax.
1.6e5
cps.108.01.5
e5
91.01.0
e5
CE=60136.2
164.2147.15.0
e4
66.4
77.0
80.0
103.0
121.989.15
0 6
0
70 8
0
90 1
00
1
1
0
12
0
1
30
14
0
150
16
0
17
0
18
0
19
0
200
2
10
2
20
2
30
2
40
2
50
2
6
0
2
70
28
0
290
30
0m/
z,
a
m
u68March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND+NHHHO
OHC2+N
Hm/z176m/z130+Nm/z103母離子為m/z130的EPI質譜碎片離子為:m/z95小結從吲哚乙酸的EPI質譜信息知,m/z176離子碎片結構為m/z772HC+N
H+Nm/z9569March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYONDm/z77m/z130m/z103m/z176,m/z190,m/z130這些母離子的質譜碎片中,都有相同 的子離子,而且離子豐度比相近,說明都有吲哚環(huán)結構,所推測 另外兩母離子結構為:NHC2HNHOO70March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND而母離子為m/z268的化合物有三個,從相應的EPI質譜圖上知,其質譜碎片大致相近,說明這三個化合物可能是同分異構體,而且其碎片離子與吲哚主結構沒有相近之處,說明三個化合物中沒有吲哚環(huán).71March,
2009,
Beijing,
China?
2009
Applied
Biosystems
Inc.
and
MDS
Inc.
Joint
OwnersABOVE
&
BEYOND1000.0
2000.0
3000.0
4000.0
5000.0
6000.07000.0
8000.0
9000.01.0e41.1e41.2e4Concentration,
ng/mLUntitled
1(176.1
/
130.2):
"Linear
Through
Zero"
Regression
("No"
weighting):
y
=
657
x
(r
=
1.0000)8.3e68.0e67.5e67.0e66.5e66.0e65.5e65.0
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