open access agilent lc/msd vl - boston university lcms...1 open access agilent lc/msd vl january...

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Open AccessOpen Access

AgilentAgilent LC/MSD VLLC/MSD VL

January 2009

CIC, MS

Chemical Instrumentation Center Chemical Instrumentation Center -- Mass SpectrometryMass Spectrometry

Instrumentation and Software

Instrumentation

� Agilent LC 1100 Series

� LC/MSD VL with ESI source

Software

� ChemStation A.10.02

� EasyAccess A.02.01

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Open Access

� Walk-up MS instrument to users 24/7

� ESI source – suitable for polar, acidic and basic molecules < 1500

m/z

� Low resolution only (1 decimal place)

� Pre-developed methods (8 and growing)

� All users are trained

� Specific methods can be developed and added


Method Types

�Flow injection analysis

� Running through LC without a

column

� Not much to tell on purity

� Confirmation of molecular ion

� Fast, run-time ~ 5 mins

� Running through LC with a

reverse phase column (C18,

2.1x50mm)

� Separation of components

� Additional info from UV data

� Run time ~ 15 mins

FIALCMS

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Open Access Methods (Positive)

0 Fragmentor100-1500100.01NoFIA_P_ACN_0Frag

30 Fragmentor100-1500100.01NoFIA_P_ACN_30Frag

120 C100-1500100.01NoFIA_P_ACN_LowT

100-1500100.01YesLCMS_P

ACN only100-1500100.005NoFIA_P_ACN

100-1500100.005NoFIA_P_HM

100-1000100.005NoFIA_P_MM

50-500100.005NoFIA_P_LM

NotesMass Range

(m/z)

Injection

Vol, (uL)

[ Conc ]

(mg/mL)

C18

ColumnMethod


Open Access Methods (Negative)

0 Fragmentor100-1500100.05NoFIA_N_ACN_0Frag

30 Fragmentor100-1500100.05NoFIA_N_ACN_30Frag

120 C100-1500100.05NoFIA_N_ACN_LowT

100-1500100.01YesLCMS_N

ACN only100-1500100.01NoFIA_N_ACN

100-1500100.01NoFIA_N_HM

100-1000100.01NoFIA_N_MM

50-500100.01NoFIA_N_LM

NotesMass Range

(m/z)

Injection

Vol, (uL)

[ Conc ]

(mg/mL)

C18

ColumnMethod

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Open Access Policy

� All users must be trained before operating this instrument.

� Suitable solvents are Methanol, Methylene Chloride, Acetonitrile or Water.

� Concentration is sample dependent, but please start at 0.005 mg/mL

(5 ppm) for FIA and 0.01 mg/mL (10 ppm) for LC/MS.

� Overloading the instrument will result in a warning and the user will also

be charged with a source-cleaning fee.

� Use 2 mL vials (insert is also approved). Fill up to at least 1/2 height.

� You do not have to, but to avoid possible carryover from previous sample,

run a blank (pure solvent). There is no charge on the blank run.

� Fail to follow these guidelines will result in removal of your permission to

operate this instrument.

� Manual direct injection users, please consult with Norman for

concentration. The highest concentration allowed is 0.5 mg/mL. Please

flush for 10 minutes after use.


Good Practice

� Before login, please check the standard spectrum to make sure the instrument is in good condition. CIC staff will perform maintenance weekly.

� You do not have to, but to avoid possible carryover from previous sample, run a blank (such as methanol). There is no charge on blank run.

� Don’t overload the machine with too concentrated sample, an ion counts between 104-105 are ideal.

� If there is a problem, please notify us ASAP so we can help.

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Data Analysis

M + 45 (Formic Acid)

M + 35 (Cl)

M + 18 (NH4)

M + 23 (Na)

M + 39 (K)

M + 41 (Acetonitrile)

ESI NegativeESI Positive

Adduct Ions

� Open Access is set up to process and print a report automatically.

� The automatic data processing is specific to the type of analysis carried out. For FIA, major peaks are reported. For LCMS, report is optimized for the most intense peaks.

� Isotope Pattern - determine a valid ion, spike or saturated signal.

� Halogen Patterns - visualize chlorine and bromine isotopes.


Common Ions for ESI+

m/z Ion Compound m/z Ion Compound

101 (M+Na)+

DMSO 257 (3M+H)+

DMSO

102 (M+H)+

triethylamine (TEA) 267 (M+H)+

tributylphosphate

104/106 (M+Cu)+

acetonitrile 273 M+

monomethoxytrityl cation (MMT)

105 (2M+Na)+

acetonitrile 279 (M+H)+

dibutylphthalate (plasticiser)

120 (M+Na+CH3CN)+

DMSO 282 plasticizer in polyethylene

122 (M+H)+

Tris 301 (M+Na)+


123 (M+H)+

dimethylaminopyridine (DMAP) 317 (M+K)+


130 (M+H)+

diisopropylethylamine (DIPEA) 336 (M+H)+

tribuyl tin formate

137 (M+ACN+NH4)+

DMSO 338 (M+H)+

erucamide

144 (M+H)+

tripropylamine (TPA) 360 (M+Na)+

erucamide

145/147 (2M+Cu)+


polysiloxane, followed by 388

146 (3M+Na)+


diisooctyl phthalate (plasticiser)

150 (M+H)+

phenyldiethylamine 413 (M+Na)+


153 (M+H)+

1,8-diazabicyclo[5,4,0]undec-7-ene(DBU) 425 (M+Na)+

unidentified contaminant (plasticiser)

157 (2M+H)+

DMSO 429 (M+K)+


159 (M+Na)+

sodium trifluoroacetate 445 (M+H)+

polysiloxane, followed by 462

179 (2M+Na)+

DMSO 449 (2M+H)+

dicyclohexyl urea (DCU)

186 (M+H)+

tributylamine 454 (M+Na+CH3CN)+


214 unknown surfactant 522 unknown

217 unidentified contaminant 550 unknown

225 (M+H)+

dicyclohexyl urea (DCU) 798 (2M+NH4)+


231 (M+NH3)+

unknown surfactant 803 (2M+Na)+


239/241 [(M.HCl)2-Cl]+

triethylamine (TEA) PEG polymer 44 amu apart

242 M+

tetrabutylammonium(C4H9)4N+

243 M+

trityl cation (New Objective Technical Note PV-3)

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Agilent Easy Access


Agilent Easy Access

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Agilent Easy Access


Agilent Easy Access

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Data Delivery

� A report is printed

� Data are saved


CIC Website

www.bu.edu/chemistry/cic/spectrometry

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