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ACQUITY UPLC 光电二极管矩阵和可调紫外可见(TV)检测器.pdf

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1、?2006 Waters Corporation?!?#$?2006 Waters Corporation?%?&?2006 Waters Corporation?(?!?#$?)?*?2006 Waters Corporation?(?!?#$?+?*?,-.?2006 Waters Corporation?,?2006 Waters Corporation?/0 1 2?3?,)?2?2006 Waters Corporation?4?&?2000 hr lamp with Lamp Optimization2000 hr lamp NO Lamp OptimizationNew Lamp

2、2000 hr lamp with Lamp Optimization?2006 Waters Corporation?5?5?5?5?2006 Waters Corporation?5?6?7?0?5?6?5?5?5?)8?TeflonAFTeflonAF?2006 Waters Corporation?)225?.?5?,.225?,9?:?(?;?5?5?2006 Waters Corporation?10 mm500 nL25 mm2400 nL?2006 Waters Corporation?)?22?.?,.?22?,9?2006 Waters Corporation?:?(?;?

3、5?5?5?2006 Waters Corporation?,59 4?AU-0.100.000.100.200.300.400.50Minutes0.000.501.001.502.002.503.00UPLC?:ACQUITY UPLC(BSM,SM,TUV)?:2.1 X 50 mm BEH C18,1.7 m?:7:3?/?+0.1%?:0.65 mL/min?:2 L?=75%?/25%?(250 uL)?=5%?/95%?(1000 uL)?:10 C?:35 C?:ACQUITY TUV 231nm(0-1.7 min)280 nm(1.7 3.0 min)20 pps,FTC=

4、0.30?=080 mg/mL2,4-D in 50%ACN/50%Water?:Empower 2?2006 Waters Corporation?AU0.00000.00050.00100.00150.00200.00250.00300.00350.00400.00450.00500.00550.0060Minutes0.300.400.500.600.700.800.901.001.101.201.301.401.501.601.70?299568452.29?236851232.16)-9 8?2.02 sec2.14 sec1.059?:?=0.000015 AU?=0.000012

5、 AU?2006 Waters Corporation?5?2006 Waters Corporation?4?5?)?!#$?5?UPLC?:ACQUITY UPLC(BSM,SM,TUV)?:2.1 X 50 mm BEH C18,1.7 m?:50%of A:10 mMol Ammonium Bicarbonate pH=1050%of B:Acetonitrile?:1.2 mL/min?:1 L(5 uL Loop,30 uL PEEK Needle,PLUNO,1 uL air gaps)?=75%ACN/25%Water(250 uL)?=50%ACN/25%Water(1000

6、 uL)?:15 C?:45 C?:ACQUITY TUV 301 nm,Various data rates,FTC=Off?=0.05 mg/mL Benzocaine,Butamben,and Tetracainein 1:1 Buffer/ACN?:Empower 21 Point per Second2 Points per Second5 Points per Second10 Points per Second20 Points per Second40 Points per Second80 Points per SecondAU0.000.050.100.150.200.25

7、0.300.350.400.450.50Minutes0.120.140.160.180.200.220.240.260.280.300.320.340.360.380.400.420.440.460.48?2006 Waters Corporation?2006 Waters Corporation?AU0.001.002.003.00Minutes0.0010.0020.0030.0040.0050.0060.0070.00?:ACQUITY UPLC TUV?:A-MethanolB-Methanol+Propyl Paraben125 mg/mL with Analytical Flo

8、w Cell50 mg/mL with High Sensitivity Flow Cell?:1-61%B in 2.5%Steps over 3 minutes?:1 mL/min?:4000 psi restrictor?:254 nm 10 pps 0.20 sec TC?2006 Waters Corporation?4?=?2006 Waters Corporation?,?:?6?0?2006 Waters Corporation?2006 Waters Corporation?2006 Waters Corporation?2006 Waters Corporation?200

9、6 Waters Corporation?-9 A-9 A)9!?#$-B)-B,.,9?#$)-)-,+,?#$)-B)-.)9)?#$B-BB9-A.?#$?86&?86&?,.4.?5 Hz40 Hz?2006 Waters Corporation?).?,.4.?%?C-?,-.D,-9D)-A.D)-B+D)-.D)-9 D)D?!?#$9?#$,?#$)?#$?.?#$,?#$)?#$?2006 Waters Corporation?%?2006 Waters Corporation?01020304050607002468101214TimePeak Intensity?:?7?

10、E?F 0?F?2006 Waters Corporation?01020304050607002468101214TimePeak Intensity?0 F G?H?E?F 0?F?2006 Waters Corporation?01020304050607005101520253035TimeAbsorbance?2006 Waters Corporation?01020304050607005101520253035TimeAbsorbance?2006 Waters Corporation?01020304050607005101520253035TimeAbsorbance?200

11、6 Waters Corporation?)!9)-A-,.)AA.)-)-,)!)-9!-).,B.,)-A-),BA),-+-.,.+!,-!+-,.?2006 Waters Corporation?&?I?)?6?6?I?)?6?J,?&?I?)?6?J 9?!?#?2006 Waters Corporation?,.?.?&?5?6?5?&?2006 Waters Corporation?2006 Waters Corporation?4?:1?2/?,-,-9,-B)9?2 1?0?.-!-)+,-.9 A?2 1?0?9,-+-B,-.9?2 1?0?+9.9 9AA-A.9,-,

12、+:1?2/?)+-9-,A,-,)?2 1?0?,9-)-.9,-)B9?2 1?0?)&0 F?4?4?0?86?0?0 2?0?1?2?1?HUPLC?:ACQUITY UPLC?TUV?:2.1 X 100 mm ACQUITY UPLC BEH C18,1.7 m?A:10 mMol?pH=10B:?:0.6 mL/min?:Time%A%B Profile0 80 20-3.0 25 7563.5 80 206?:1 L?=75%?/25%?(1000 uL)?=50%?/25%?(3000 uL)?:15 C?:40 C?:ACQUITY TUV 290 nm,20 pps,FT

13、C=0.10?=0.125 mg/mL Butamben in 75%ACN/25%Water?:Empower 2 CDS?2006 Waters Corporation?C-22R(epimer B)C-22S(epimer A)AU0.000.050.100.150.200.250.300.350.400.450.500.550.600.650.700.75Minutes0.501.001.502.002.503.003.504.004.505.005.506.006.507.007.508.00?UPLC?:ACQUITY UPLC?:2.1 X 100 mm BEH C18,1.7

14、m?A:10 mmoL?pH 3.2/?68:32?B:?:0.60 mL/min?:3 L(PLUNO 5uL Loop)?:1000 uL?/?/IPA 5:1:1?:3000 uL?/?7:3?:15 C?:45 C?:ACQUITY TUV(240 nm),20 pps,TC=0.1 sec?:Empower II?:1.0 mg/mL Budesonide in mobile phase16,17-(butylidenebis(oxy)-11,21-dihydroxy-,(11-?,16-?)-pregna-1,4-diene-3,20-dione?:1 H?0 H?Budesoni

15、de?2006 Waters Corporation?C-22R(epimer B)C-22S(epimer A)AU0.0000.0010.0020.0030.0040.0050.0060.0070.0080.0090.010Minutes0.501.001.502.002.503.003.504.004.505.005.506.006.507.007.508.00Peak#S/NArea%11200.0332380.0113690.0324100.0105300.0246510.0467280.0258160.0189890.1510 150.02211430.056121400.2013

16、10891.63C-22R 2916949.0C-22S 2634148.516140.02717200.03918110.02412938746510111213171816?97.5?:1 H?0 H?2006 Waters Corporation?44?-)8?0.01%?)-,?2?)-,?2?2006 Waters Corporation?Prilocaine(API)o-Toluidine(0.01%Impurity)R2=0.9998R2=0.998?K?!8?4),8?.8?4).8?-)8?44?-)8?2006 Waters Corporation?1.40 AU Full

17、 Scale?)2F 2?1.2 nm?1.2 nm?.)+AA-+,!9-!?B-!,-B+?L?;?),)!9-)AA)-+?L?;?)A-+)-)A?L?;?),-B)-B+?L?;?A),)-.-A9 A?L?;?!-!+!?L?;?B+,-,-B.,?L?;?+9 A-,-B A?L?;?.,-)B-+.?L?;?9!-9-.A.?L?;?A-9-.,?L?;?,A!-,-9 B?L?;?)&?8?2006 Waters Corporation?0/1 7?0?2006 Waters Corporation?:?2006 Waters Corporation?/1?0?+.-!).-

18、B?2 1?0?BB A,BAA-!9.9-9!9?/1?0?.+-9 9-+?2 1?0?+)-!,-.B?2 1?0?.,-),-9 A?2 1?0?9+-)-9 A.?2 1?0?)-9)-)B.?2 1?0?,B-9)-.?2 1?0?)&0 F?4?4?0?86?0?0 2?0?1?2?1?H?2006 Waters Corporation?0.005%Standard0.01%Standard?2006 Waters Corporation?275.0275.0275.0?(LOQ)82.582.582.5?(LOD)0.0085%0.0025%27.5Y=3.21 e+4 X+3

19、.4?C0.0049%0.0015%27.5Y=5.61 e+4 X?0.8?B0.0105%0.0029%27.5Y=2.52 e+4 X+10.3?Mass%?Mass%?(?AU)?.-!8-B8-)8?I+?:?2006 Waters Corporation?,9?,.?)?,AA+?M.?2?,AA+?)-.?2006 Waters Corporation?,AA+?2006 Waters Corporation?AU-0.00036-0.00024-0.000120.000000.00012Minutes0.000.200.400.600.801.001.201.401.601.8

20、02.00?,AA+?,AA+?2006 Waters Corporation?,AA+?,.-,9+-?$%&?%(?)(#?*?%+-?-?&,?-?,?!9-99-!)B-)-,?$%&?%(?)?*?%+(#?.?/0?/?1*?,+?K)?K-,?K,.9?2?K.?K.?20?2006 Waters Corporation?AU-0.0009-0.0008-0.0007-0.0006-0.0005-0.0004-0.0003-0.0002-0.00010.00000.00010.00020.0003Minutes0.001.002.003.004.005.006.007.008.0

21、09.00?(?=230 nm)?TUV 10 mm=0.000167 AU?TUV 10 mm=0.000028 AU?2006 Waters Corporation?2?(nm)TUVEnhanced TUV Enhanced TUV(Analytical/10 mm)(High-Sens/25 mm)1951.7720.1170.1472000.3440.0730.0542050.0940.0380.0312100.1000.0320.0282140.0910.0430.0042540.0750.0410.0172800.0740.0390.0293131.1930.0270.02042

22、00.1580.0590.0985050.2180.0900.0455400.1670.1290.068?H 0?:?0?0?2006 Waters Corporation?:?2006 Waters Corporation?:?5?,.8?2006 Waters Corporation?&7?&G?4?5?,?2006 Waters Corporation?&7?&G?4?2006 Waters Corporation?:?:?.8?.8?2006 Waters Corporation?2006 Waters Corporation?2006 Waters Corporation?2006 Waters Corporation?2006 Waters Corporation?:?:?5?2006 Waters Corporation?MBF-ONMBF-OFF?2006 Waters Corporation?2006 Waters Corporation?:?:?:?5?;?-7?2?

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