Ambient ionization explained

Ambient ionization is a form of ionization in which ions are formed in an ion source outside the mass spectrometer without sample preparation or separation.[1] [2] [3] [4] Ions can be formed by extraction into charged electrospray droplets, thermally desorbed and ionized by chemical ionization, or laser desorbed or ablated and post-ionized before they enter the mass spectrometer.[5]

Solid-liquid extraction

Solid-liquid extraction based ambient ionization is based on the use of a charged spray, for example electrospray to create a liquid film on the sample surface.[6] Molecules on the surface are extracted into the solvent. The action of the primary droplets hitting the surface produces secondary droplets that are the source of ions for the mass spectrometer.

Desorption electrospray ionization (DESI) is one of the original ambient ionization sources[7] and uses an electrospray source to create charged droplets that are directed at a solid sample. The charged droplets pick up the sample through interaction with the surface and then form highly charged ions that can be sampled into a mass spectrometer.[8]

Desorption atmospheric pressure photoionization (DAPPI) is a solid-liquid extraction ambient ionization method that enables the direct analysis of samples deposited on surfaces by means of a jet of hot solvent vapour and ultraviolet light. The hot jet thermally desorbs the sample from a surface and the vaporized sample is ionized by a vacuum ultraviolet light and consequently sampled into a mass spectrometer.[9]

Plasma-based techniques

Plasma-based ambient ionization is based on an electrical discharge in a flowing gas that produces metastable atoms and molecules and reactive ions. Heat is often used to assist in the desorption of volatile species from the sample. Ions are formed by chemical ionization in the gas phase.

One proposed mechanism involves Penning ionization of ambient water clusters in a helium discharge:

He^\ast + [(H2O)_\mathit{n}H] -> [(H2O)_{\mathit n-1}H]+ + OH^. + e^- .

The protonated water clusters can then protonate the sample molecules via

[(H2O)_\mathit{n}H]+ + M -> [M{} + H]+ + \mathitH2O.

For this ionization pathway, the gas-phase acidity of the protonated water clusters and the gas-phase basicity of the analyte molecule are of crucial importance. However, since especially smaller protonated water clusters with n = 1,2,3... exhibit very high gas-phase acidities, even compounds with a rather low gas-phase basicity are readily ionized by proton transfer, yielding [M+H]+ quasimolecular ions.[10] [11]

Besides protonated water clusters, other positively charged reagent ions, such as NO+, O2+, NO2+ and CO2+, may be formed in the afterglow region.[12] These additional reagent ions are capable of ionizing compounds via charge-transfer processes and, thus, offer alternative routes of ionization besides proton transfer, leading to a broader range of suitable analytes. Nevertheless, these ionization mechanisms may also lead to the formation of adducts and oxidation of the original analyte compounds.

Although most applications focus on the detection of positive ions, measurements in the negative mode are for most of the plasma-based ion sources also possible. In this case, reagent ions, such as O2–, can deprotonate the analyte molecules to give [M–H]– quasimolecular ions, or form adducts with species such as NO3–, yielding [M+NO<sub>3</sub>]– ions. Measurements in the negative ion mode are especially favorable when the analyte molecules exhibit a high gas-phase acidity, as it is the case e.g. for carboxylic acids.

One of the most used plasma-based techniques for ambient ionization is probably Direct analysis in real time (DART), since it is commercially available. DART is an atmospheric pressure ion source that operates by exposing the sample to a gas stream (typically helium or nitrogen) that contains long-lived electronically or excited neutral atoms, vibronically excited molecules (or "metastables"). Excited states are formed in a glow discharge in a chamber through which the gas flows.[13]

Laser assisted

Laser-based ambient ionization is a two-step process in which a pulsed laser is used to desorb or ablate material from a sample and the plume of material interacts with an electrospray or plasma to create ions. Lasers with ultraviolet and infrared wavelengths and nanosecond to femtosecond pulse widths have been used. Although atmospheric pressure MALDI is performed under ambient conditions,[14] it is not generally considered to be an ambient mass spectrometry technique.[15] [16]

Laser ablation was first coupled with mass spectrometry in the 1980s for the analysis of metals using laser ablation inductively coupled plasma mass spectrometry (LA-ICPMS).[17] The laser ablates the sample material that is introduced into an ICP to create atomic ions.

Infrared laser desorption can be coupled with atmospheric pressure chemical ionization using laser desorption atmospheric pressure chemical ionization (LD-APCI).[18] For ambient ionization with a spray, the sample material is deposited on a target near the spray. The laser desorbs or ablates material from the sample that is ejected from the surface and into the spray, which can be an APCI spray with a corona discharge or an electrospray. Ambient ionization by electrospray-assisted laser desorption/ionization (ELDI) can be accomplished with ultraviolet[19] and infrared lasers[20] to the desorb material into the electrospray plume. Similar approaches to laser desorption/ablation into an electrospray are matrix-assisted laser desorption electrospray ionization (MALDESI),[21] laser ablation electrospray ionization (LAESI),[22] laser assisted desorption electrospray ionization (LADESI), laser desorption electrospray ionization (LDESI),[23] [24] laser ablation mass spectrometry (LAMS),[25] and laser desorption spray post-ionization (LDSPI).[26] The term laser electrospray mass spectrometry has been used to denote the use of a femtosecond laser for ablation.[27] [28] Laser ablation into an electrospray produces highly charged ions that are similar to those observed in direct electrospray.

An alternative ionization approach following laser desorption is a plasma. UV laser ablation can be combined with a flowing afterglow plasma for mass spectrometry imaging of small molecules. and IR desorption has been combined with a metastable ion source.

Two step non-laser

In two-step non-laser methods, the material removal from the sample and the ionization steps are separate.

Probe electrospray ionization (PESI) is a modified version of conventional electrospray ionization in which the capillary for sample solution transferring is replaced by a solid needle with a sharp tip.[29] Compared with conventional electrospray ionization, high salt tolerance, direct sampling, and low sample consumption are found with PESI. PESI is not a continuous process; the needle for sampling and spraying is driven up and down at a frequency of 3–5 Hz.

Vapor-ion, charge transfer reaction

The analytes are in the vapor phase. This includes breath, odors, VOCs, and other molecules with low volatility that, due to the constant improvements in sensitivity, are detectable in the vapor phase despite their low vapor pressure. Analyte ions are produced via gas-phase chemical reactions, where charging agents collide with the analyte molecules and transfer their charge. In secondary electro-spray ionization (SESI), a nano-electrospray operated at high temperature produces nanodroplets that evaporate very rapidly to produce ions and protonated water clusters that ionize the vapors of interest. SESI is commonly used for the analysis of trace concentrations of vapors being able to detect low volatility species in the gas phase with molecular masses of up to 700 Da.

Table of techniques

In the table below, ambient ionization techniques are classified in the categories "extraction" (a solid or liquid extraction processes dynamically followed by spray or chemical ionization), "plasma" (thermal or chemical desorption with chemical ionization), "two step" (desorption or ablation followed by ionization), "laser" (laser desorption or ablation followed by ionization), "acoustic" (acoustic desorption followed by ionization), multimode (involving two of the above modes), other (techniques that do not fit into the other categories).

AcronymTechniqueClassification
AFAI[30] Air flow-assisted ionizationExtraction
AFADESI[31] Air flow-assisted desorption electrospray ionizationExtraction
APGDDI[32] Atmospheric pressure glow discharge desorption ionizationPlasma
APPIS[33] Ambient pressure pyroelectric ion source
APTDCI[34] Atmospheric pressure thermal desorption chemical ionization Two-step
APTDI[35] Atmospheric pressure thermal desorption/ionizationPlasma
ASAP[36] Atmospheric pressure solids analysis probePlasma
BADCI[37] Beta electron-assisted direct chemical ionizationTwo step
CALDI[38] Charge assisted laser desorption/ionizationLaser
DAPCI[39] Desorption atmospheric pressure chemical ionizationPlasma
DAPPI[40] Desorption atmospheric pressure photoionizationExtraction
DART[41] Direct analysis in real timePlasma
DBDI[42] Dielectric barrier discharge ionizationPlasma
DCBIDesorption corona beam ionizationPlasma
DCIDesorption chemical ionizationPlasma
DEFFI[43] Desorption electro-flow focusing ionizationExtraction
DEMI[44] Desorption electrospray/metastable-induced ionizationMultimode
DESIDesorption electrospray ionizationExtraction
DeSSI[45] Desorption sonic spray ionizationExtraction
DICE[46] Desorption ionization by charge exchangeExtraction
DIP-APCI[47] Direct inlet probe–atmospheric-pressure chemical ionization Two-step
DPESI[48] Direct probe electrospray ionization
EADESI[49] Electrode-assisted desorption electrospray ionizationExtraction
EASI[50] Easy ambient sonic-spray ionizationExtraction
EESI[51] Extractive electrospray ionizationTwo step
ELDI[52] Electrospray laser desorption ionizationLaser
ESA-Py[53] Electrospray-assisted pyrolysis ionizationSpray
ESTASI[54] Electrostatic spray ionizationExtraction
FAPA[55] Flowing atmospheric pressure afterglowPlasma
FIDI[56] Field-induced droplet ionization
HALDI[57] High-voltage-assisted laser desorption ionizationLaser
HAPGDIHelium atmospheric pressure glow discharge ionizationPlasma
IR-LAMICI[58] Infrared laser ablation metastable-induced chemical ionizationLaser
JeDI[59] Jet desorption electrospray ionizationExtraction
LADESI[60] Laser assisted desorption electrospray ionizationLaser
LAESI[61] Laser ablation electrospray ionizationLaser
LA-FAPA[62] Laser ablation flowing atmospheric pressure afterglowLaser
LA-ICP[63] Laser ablation inductively coupled plasmaLaser
LD-APCILaser desorption atmospheric pressure chemical ionizationLaser
LDTD[64] Laser diode thermal desorptionLaser
LDESILaser desorption electrospray ionizationLaser
LDSPILaser desorption spray post-ionizationLaser
LEMSLaser electrospray mass spectrometryLaser
LESA[65] Liquid extraction surface analysisExtraction
LIAD-ESI[66] Laser-induced acoustic desorption-electrospray ionizationAcoustic
LMJ-SSP[67] Liquid microjunction-surface sampling probeExtraction
LPTD[68] Leidenfrost phenomenon-assisted thermal desorptionTwo-step
LS-APGD[69] Liquid sampling-atmospheric pressure glow discharge Plasma
LSI[70] Laser spray ionizationOther
LTP[71] Low temperature plasmaPlasma
MAII[72] Matrix-assisted inlet ionizationOther
MALDESI[73] Matrix-assisted laser desorption electrospray ionizationLaser
MFGDP[74] Microfabricated glow discharge plasma Plasma
MIPDI[75] microwave induced plasma desorption ionizationPlasma
nano-DESI[76] Nanospray desorption electrospray ionizationExtraction
ND-EESI[77] Neutral desorption extractive electrospray ionizationTwo step
PADI[78] Plasma-assisted desorption ionizationPlasma
Paint Spray*[79] Paint sprayExtraction
PALDI[80] Plasma-assisted laser desorption ionizationLaser
PAMLDI[81] Plasma-assisted multiwavelength laser desorption ionizationLaser
PASIT[82] Plasma-based ambient sampling/ionization/transmissionExtraction
PAUSI[83] Paper assisted ultrasonic spray ionization
PESI[84] Probe electrospray ionizationTwo step
PS[85] Paper spray
PTC-ESI[86] Pipette tip column electrospray ionizationExtraction
RADIO[87] Radiofrequency acoustic desorption and ionizationAcoustic
RASTIR[88] Remote analyte sampling transport and ionization relay
REIMS[89] Rapid evaporative ionization mass spectrometryOther
RoPPI[90] Robotic plasma probe ionizationTwo-step
SACI[91] Surface activated chemical ionization
SAII[92] Solvent-assisted inlet ionizationOther
SAWN[93] Surface acoustic wave nebulizationAcoustic
SESI[94] Secondary electrospray ionizationVapor-ion, charge transfer
SPA-nanoESI[95] Solid probe assisted nanoelectrospray ionizationTwo-step
SPAMS[96] Single-particle aerosol mass spectrometryOther
SSI[97] Sponge-Spray Ionization
SSP[98] Surface sampling probeExtraction
SwiFerr[99] Switched ferroelectric plasma ionizerOther
TDAMS[100] Thermal desorption-based ambient mass spectrometrySpray
TM-DESI[101] Transmission mode desorption electrospray ionizationExtraction
TS[102] Touch sprayTwo-step
UASI[103] Ultrasonication-assisted spray ionizationAcoustic
V-EASI[104] Venturi easy ambient sonic-spray ionizationExtraction
BS [105] Brush-Spray IonizationTwo-step
FS [106] Fiber-Spray Ionization Extraction
(*) Not an acronym.

Table of commercially available ambient ionization sources

!Technique!Commercial Brand!Company !Website
Ambient Pressure Photo Ionization (APPI)MasCom

GC-(APPI)

MasCom Technologies GmbHhttps://www.mascom-bremen.de/
Atmospheric pressure solids analysis probe (ASAP)RADIANWaters, USAhttps://www.waters.com/
Desorption Electrospray Ionization (DESI)DESI2DProsolia Inc, Indianapolis, INhttps://prosolia.com/
Direct Analysis in Real Time (DART)DARTIonSense Inc, Saugus, MAhttps://www.ionsense.com/
Liquid Extraction Surface Analysis (LESA)TriVersaNanoMateAdvion, Ithaca, NYhttps://advion.com/
Probe Electrospray Ionization (PESI)DPiMS-8060Shimadzu, Japanhttps://www.shimadzu.com/
Rapid evaporative Ionization Mass Spectrometry (REIMS)REIMSWaters, USAhttps://www.waters.com/
Secondary Electrospray Ionization (SESI)SUPER SESIFossil Ion Technology, Spainhttps://www.fossiliontech.com/
Soft Ionization by Chemical Reaction In Transfer (SICRIT)SICRITPlasmion GmbH, Germanyhttps://plasmion.com/

Notes and References

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