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Determination of five effective components in medicinal material of Tripterygium by UPLC-ESI-MS/MS

超高效液相色谱串联质谱同时测定雷公藤药材中5个有效成分



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Determinationoffiveefectivecomponentsinmedicinalmaterialof
TripterygiumbyUPLCESIMS/MS
HUJun1,2,LIUChao1,GUOLanping1,HAOQingxiu1,KANGLiping1,NANTiegui1,
LIUYong2,ZHANZhilai1,HUANGLuqi1
(1StateKeyLaboratoryofDaodiHerbsBreedingBase,NationalResourceCenterforChineseMateriaMedica,
ChinaAcademyofChineseMedicalSciences,Beijing100700,China;
2SchoolofChineseMateriaMedica,BeijingUniversityofChineseMedicine,Beijing100102,China)
[Abstracts] Thispaperisaimedtodevelopamethodforthedeterminationoffiveefectivecomponentsinmedicinalmaterialof
Tripterygiumusingultraperformanceliquidchromalographycoupledwithelectrosprayionizationtandemmassspectrometry(UPLCESI
MS/MS),whichthenwasusedtostudytheircontentsinrawmaterialsfromdiferentareasanddiferentsourcesTheseparationwas
performedonaWatersACQUITYUPLCCSHC18Scolumn(21mm×100mm,17μm),usingacetonitrile02% ammoniumforma
teaqueoussolutionasmobilephaseThetargetcomponentsweredetectedinmultiplereactionmonitoring(MRM)modebymassspec
trometrywithelectrosprayionization(ESI)sourceoperatedinpositiveionizationmodeThequantitativeresultsshowedthatgoodline
aritywasachievedintheirrespectivelinearrangesandfinedeterminationcoeficient(r>09978),andtheoveralrecoveriesranged
from9672%1032% withtheRSDrangingfrom10%24%Themethodissensitiveandaccurate,andsuitablefortheefectivecom
ponentsquantificationinmedicinalmaterialofTripterygium;contentsoffiveefectivecomponentsfromdiferentsourcesvarysignifi
·9641·
2016
y

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41
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Vol41,No.8 April,2016
cantly,sothequalityandsafetyofmedicinalmaterialofTripterygiumneedstobeimprovedItisveryimportanttocontrolthequality
withmultiindexforclinicsafety
[Keywords] UPLCESIMS/MS;Tripterygiumwilfordi;Tripterygiumhypoglaucum;efectivecomponents;contentdetermination
doi:10.4268/cjcmm20160817
  
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Table1 Sourceofmaterials
No.
,X 9: (>F

VDW
Tripterygiumwilfordi
pKݯ
 

VDW

>?
) Twilfordi(cultivated)
9ßp
 

VDW
Twilfordi
Cb¹£
 

΁yHÙ
Thypoglaucum
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Thypoglaucum
pKá_
 
10
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11
΁yHÙ
Thypoglaucum
9[É
 
12
VDW

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) Twilfordi(cultivated)
Cb¹£
 
13
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Table2 OptimizedMS/MSparameters
_HÉ
tR/min !¹ª-¶ m/z ùæUÆ/V ®¯UÆ/eV ®¯þåÁUÆ/eV
VDWæF
  111 361/145 160 35 13
VDW8ýF
180 359/143 140 40 14
VDW!Ÿ
  297 884/838 30 42 13
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  303 858/840 264 37 14
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Fig1 MRM of5componentsinTripterygiumwilfordiand
T.hypoglaucum
T

,ʵÄÉʖ

Q©Ù=»§¹ò9

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渋Œ¶#[NP“v‘•
(S/N)
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šé

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(LOD),
l+
3。
·1741·
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41
âÓ

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Vol41,No.8 April,2016
+
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Table3 Calibrationcurves,LODs,andLOQsof5components
ʵ Éʖ

§¹ò9
/μg·L-1 !õC/μg·L-1 ¨©C/μg·L-1
VDWæF
  Y=406248X+319786 09993 599~76667 149 002
VDW8ýF
Y=345379X+63797 09998 365~46667 365 011
VDW!Ÿ
  Y=302922X+2296759 09991 26563~17000 111 069
VDW¾Ÿ
  Y=564E+4X+506E+6 09986 26563~17000 003 004
VDWŠŸ
  Y=2915964X+192E+6 09978 8474~5400 029 009
243 
]+r

m!¹

;u¹»É”˜B.
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]+rB.
 
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NP

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21
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17%~26%,
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;u¹B.
 
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#

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©!xʵxõÄ
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¦
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+#;u¹Þ

2433 
m!¹B.
 
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/B[NP

ˆ
21
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8,12,24h
‘&µî

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ä+/B[NPþ‰À¦
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8m!

2434 
ɔ˜B.
 
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&[

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020g,
]+‘i±

$

O

Y“rÄ

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ˆ
21
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DM

YʵÄ͑‘
&ɔ˜¦
9672% ~1032%,
®
RSD
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10% ~
24%,
+#ɔ˜Þ

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4。
+
4 
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;u¹

m!¹»‘&ɔ˜
(n=6)
Table4 Precision,repeatability,stability,andrecoveryof5
components(n=6) %
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RSD
‘&ɔ˜
]+r ;u¹ m!¹ ͑ɔ˜
RSD
VDWæF
  20 42 28 9672 24
VDW8ýF
26 25 28 9903 13
VDW!Ÿ
  17 34 14 1032 15
VDW¾Ÿ
  22 40 13 1012 10
VDWŠŸ
  17 25 29 9823 20
25 
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VDW­ÎyHÙ,X$

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Table5 Determinationof5componentsinTripterygiumwilfor
diandThypoglaucum μg·g-1
No
VDW
æF
VDW
8ýF
VDW

VDW
¾Ÿ
VDW
ŠŸ
1 0090 0043 12255 0774 1650
2 0043 0012 7824 0070 0168
3 0069 0011 2507 3392 1796
4 0048 0001 1270 0735 0267
5 0083 0011 4041 0992 2177
6 0075 0019 16440 0140 0561
7 0047 0019 8261 0486 1182
8 0102 0047 11679 0658 1848
9 0032 0012 16920 0143 0532
10 0087 0021 5105 2931 1227
11 0053 0075 3452 0744 1157
12 0052 0015 5219 4611 4527
13 0044 0014 2457 0870 0487
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