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NASA NTRS2015

Microelectrospray Thrusters

Propulsion technology is often a critical enabling technology for space missions. NASA is investing in technologies to enable high value missions with very small spacecraft, even CubeSats. However, these nanosatellites currently lack any appreciable propulsion capability. CubeSats are typically deployed and tumble or drift without any ability to transfer to higher value orbits, perform orbit maintenance, or perform de-orbit. Larger spacecraft can also benefit from high precision attitude control systems. Existing practices include reaction wheels with lifetime concerns and system level complexity. Microelectrospray thrusters will provide new propulsion capabilities to address these mission needs. Electric propulsion is an approach to accelerate propellant to very high exhaust velocities through the use of electrical power. Typical propulsion systems are limited to the combustion energy available in the chemical bonds of the fuel and then acceleration through a converging diverging nozzle. However, electric propulsion can accelerate propellant to ten times higher velocities and therefore increase momentum transfer efficiency, or essentially, increase the fuel economy. Fuel efficiency of thrusters is proportional to the exhaust velocity and referred to as specific impulse (Isp). The state-of-the-art (SOA) for CubeSats is cold gas propulsion with an Isp of 50-80 s. The Space Shuttle main engine demonstrated a specific impulse of 450 s. The target Isp for the Mars Exploration Program (MEP) systems is >1,500 s. This propellant efficiency can enable a 1-kg, 10-cm cube to transfer from low-Earth orbit to interplanetary space with only 200 g of propellant. In September 2013, NASA's Game Changing Development program competitively awarded three teams with contracts to develop MEP systems from Technology Readiness Level-3 (TRL-3), experimental concept, to TRL-5, system validation in a relevant environment. The project is planned for 18 months of system development. Due to the ambitious project goals, NASA has awarded contracts to mature three unique methods to achieve the desired goals. Some of the MEP concepts have been developed for more than a decade at the component level, but are now ready for system maturation. The three concepts include the high aspect ratio porous surface (HARPS) microthruster system, the scalable ion electrospray propulsion system (S-iEPS), and an indium microfluidic electrospray propulsion system. The HARPS system is under development by Busek Co. The HARPS thruster is an electrospray thruster that relies on surface emission of a porous metal with a passive capillary wicking system for propellant management. The HARPS thruster is expected to provide a simple, high ΔV and low-cost solution. The HARPS thruster concept is shown in figure 1. Figure 1 includes the thruster, integrated power processing unit, and propellant reservoir.

Dankanich, John↗
NASA NTRS1995

Spray combustion at normal and reduced gravity in counterflow and co-flow configurations

Liquid fuel dispersion in practical systems is typically achieved by spraying the fuel into a polydisperse distribution of droplets evaporating and burning in a turbulent gaseous environment In view of the nearly insurmountable difficulties of this two-phase flow, a systematic study of spray evaporation and burning in configurations of gradually increasing levels of complexity, starting from laminar sprays to fully turbulent ones, would be useful. A few years ago we proposed to use an electrostatic spray of charged droplets for this type of combustion experiments under well-defined conditions. In the simplest configuration, a liquid is fed into a small metal tube maintained at several kilovolts relative to a ground electrode few centimeters away. Under the action of the electric field, the liquid meniscus at the outlet of the capillary takes a conical shape, with a thin jet emerging from the cone tip (cone-jet mode). This jet breaks up farther downstream into a spray of charged droplets - the so-called ElectroSpray (ES). Several advantages distinguish the electrospray from alternative atomization techniques: (1) it can produce quasi-monodisperse droplets over a phenomenal size range; (2) the atomization, that is strictly electrostatic, is decoupled from gas flow processes, which provides some flexibility in the selection and control of the experimental conditions; (3) the Coulombic repulsion of homopolarly charged droplets induces spray self-dispersion and prevents droplet coalescence; (4) the ES provides the opportunity of studying regimes of slip between droplets and host gas without compromising the control of the spray properties; and (5) the compactness and potential controllability of this spray generation system makes it appealing for studies in reduced-gravity environments aimed at isolating the spray behavior from natural convection complications. With these premises, in March 1991 we initiated a series of experiments under NASA sponsorship (NAG3-1259 and 1688) in which the ES was used as a research tool to examine spray combustion in counter-flow and co-flow spray diffusion flames, as summarized below. The ultimate objective of this investigation is to examine the formation and burning of sprays of liquid fuels, at both normal and reduced gravity, first in laminar regimes and then in turbulent ones.

Gomez, Alessandro↗
NASA NTRS2010

Three Methods of Detection of Hydrazines

Three proposed methods for measuring trace quantities of hydrazines involve ionization and detection of hydrazine derivatives. These methods are intended to overcome the limitations of prior hydrazine- detection methods. Hydrazine (Hz), monomethylhydrazine (MMH), and unsymmetrical dimethylhydrazine (UDMH) are hypergolic fuels and are highly reactive, toxic, and corrosive. A capability to measure concentrations of hydrazines is desirable for detecting leaks and ensuring safety in aerospace settings and in some industrial settings in which these compounds are used. One of the properties (high reactivity) that make it desirable to detect trace amounts of hydrazines also makes it difficult to detect hydrazines and measure their concentrations accurately using prior methods: significant amounts are lost to thermal and catalytic decomposition prior to detection. Further complications arise from the sticky nature of hydrazines: Sample hydrazine molecules tend to become irreversibly adsorbed onto solid surfaces with which they come into contact during transport to detectors, giving rise to drift in detector responses. In each proposed method, the reactive, sticky nature of hydrazines would be turned to advantage by providing a suitably doped substrate surface with which the hydrazines would react. The resulting hydrazine derivatives would be sufficiently less sticky and sufficiently more stable so that fewer molecules would be lost to decomposition or adsorption during transport. Consequently, it would be possible to measure concentration with more sensitivity and less error than in prior techniques. The first proposed method calls for the use of a recently developed technique known as desorption electrospray ionization (DESI), in which a pneumatically assisted micro -electrospray at ambient pressure is directed at a surface of interest. In this case, the surface of interest would be that of a substrate described above.

Griffin, Timothy↗
NASA NTRS2015

20-mN Variable Specific Impulse (Isp) Colloid Thruster

Busek Company, Inc., has designed and manufactured an electrospray emitter capable of generating 20 mN in a compact package (7x7x1.7 in). The thruster consists of nine porous-surface emitters operating in parallel from a common propellant supply. Each emitter is capable of supporting over 70,000 electrospray emission sites with the plume from each emitter being accelerated through a single aperture, eliminating the need for individual emission site alignment to an extraction grid. The total number of emission sites during operation is expected to approach 700,000. This Phase II project optimized and characterized the thruster fabricated during the Phase I effort. Additional porous emitters also were fabricated for full-scale testing. Propellant is supplied to the thruster via existing feed-system and microvalve technology previously developed by Busek, under the NASA Space Technology 7's Disturbance Reduction System (ST7-DRS) mission and via follow-on electric propulsion programs. This project investigated methods for extending thruster life beyond the previously demonstrated 450 hours. The life-extending capabilities will be demonstrated on a subscale version of the thruster.

Demmons, Nathaniel↗
NASA NTRS2020

Life-Limiting Factors of the CMTS for Precision Pointing Observatory Missions

Development of the next generation Colloid Micronewton Thruster System (CMTS) has focused on incorporation of complete redundancy, and extension of life beyond the 3,458 hrs previously demonstrated to the >40,000 hrs necessary for future missions. The present life- limiting factor of the CMTS is impingement of the electrospray beam onto the electrostatic grids, which is mitigated by the use of porous grid structures to adsorb and trap the small fraction (typically <0.5%) of the beam that intercepts the grids. A detailed alignment survey using a single emitter electrospray source has been performed in order to establish thruster production requirements and produce data necessary for lifetime model validation. Capillary emitter tilt (Θ), lateral displacement (X), and source spacing (Z), where independently assessed for their impact on changes in grid interception, as well as combined lateral and tilt displacement. Throughout testing, incremental improvements were made to reduce facility effects that impacted measured results. The data validate the alignment tolerances used in design and fabrication of the CMTS. Increased interception was not observed until emitter tilt exceeded 3X, lateral misalignment exceeded 5X, and emitter spacing >1.5X tolerance requirements. Results also indicate that, at target grid impingement levels <0.5%, facility effects begin to dominate measured grid currents and must be mitigated for more accurate assessments of thruster life.

Ziemer, John K.↗
NASA NTRSDate not supplied

Design, Analysis, Testing, and Flight Activities for A Green Propulsion Dual Mode (Gpdm) Technology Demonstration Mission

NASA’s Strategic Plan (2022) outlines specific technology development objectives which direct the Agency to “innovate and advance transformational space technologies.” An example of these potentially high-impact space technologies is the low-toxicity or “green” rocket propellant known as ASCENT (or Advanced Spacecraft Energetic Non-Toxic Propellant). Developed in the 2010’s by the Air Force Research Lab (AFRL), ASCENT (formerly AF-315E) has shown improved specific impulse density (50% higher) vs. hydrazine in addition to its favorable in-space storability and ease of handling capability. The chemical propulsion capability of ASCENT has been demonstrated on several missions including the Green Propulsion Infusion Mission (GPIM) in 2019 and most recently, the Lunar Flashlight mission. ASCENT is an ionic liquid, which lends itself as both a chemical and an electrospray propellant. The capability to use the same propellants in multiple modes using the same propellant tank and feed system has yet to be demonstrated in orbit. This capability, if proven successful has the potential to reduce system weight and complexity, while taking advantage of both high thrust and high propellant efficiency in electrospray mode. The GPDM Project, managed by the Marshall Space Flight Center is seeking to develop a dual-mode propulsion system as the payload on a small spacecraft (6U CubeSat) and subsequent in-space demonstration. This paper will summarize the concept, ground testing as well as mission operations plan for demonstrating green “dual-mode” propulsion.

Nehemiah J. Williams↗
NASA NTRSDate not supplied

A Green Propulsion Dual Mode (GPDM) In-Space Technology Demonstration on a 6U CubeSat

Over the past decade there has been an increase in the launch and operations of small spacecraft. Small spacecraft (defined as having a total vehicle mass of < 180 kg) provide an opportunity for low-cost, high impact technology demonstrations on a small scale. They also create opportunities for government, industry, and academic to engage, transfer knowledge, and extend partnerships with non-traditional partners. NASA’s Marshall Space Flight Center (MSFC) is leading a collaborative effort to demonstrate a dual-mode (chemical and electrospray) propulsion system using a common propellant system as a payload on a 6U CubeSat. The novel feature in the propulsion system is the interfacing of propulsion technologies requiring dramatically different operating conditions and support hardware. GPDM will use a low toxicity or “green” propellant known as Advanced Spacecraft Energetic Non-Toxic (ASCENT) to demonstrate using a chemical thruster for translation burns and electrospray propulsion for both attitude control and translational burns on the spacecraft. Specific mission activities could include demonstration of collision avoidance during frequent altitude adjustment maneuvers to validate thruster performance and managing extended duration thruster burns of at least 24 hours with limited vehicle contact times. This paper will summarize the ground testing, spacecraft development, mission objectives, and mission planning activities to achieve some of GPDM’s technical objectives.

Nehemiah Joel Williams↗
NASA NTRSDate not supplied

Mission Architecture for the Green Propulsion Dual Mode Mission

Current spacecraft propulsion technologies are broadly divided into chemical and electric propulsion modes, each of which has unique advantages. It is common for both systems to have a place in interplanetary spacecraft, but the size, weight, and power required to carry two separate propulsion systems is extremely limiting for small spacecraft such as CubeSats. The upcoming NASA STMD-funded Green Propulsion Dual Mode (GPDM) mission will demonstrate on-orbit a novel dual-mode propulsion system known as the GPDM Propulsion System that uses the AF-M315E/ASCENT green monopropellant to feed both a chemical 100 mN monopropellant thruster and four electrospray thrusters. GPDM will fly a 6U CubeSat in low Earth orbit and perform orbit-raising and lowering maneuvers to characterize the performance of this dual-mode propulsion technology, enabling a new generation of future interplanetary small satellite explorers. The Georgia Institute of Technology Space Systems Design Laboratory (SSDL) is conducting the design, assembly, integration, testing, and mission operations of the GPDM host spacecraft, as well as the integration of the GPDM Propulsion System payload, designed by NASA’s Marshall Spaceflight Center (MSFC). The NASA Marshall Space Flight Center is overseeing the overall GPDM project as well as specific technology development activities of the GPDM Propulsion System, while electrospray thrusters are supplied by the MIT Space Propulsion Lab, with additional components supplied by MMA Design, Blue Canyon Technologies, Quasonix, Xiphos, and Rubicon Space Systems. The GPDM spacecraft will carry the GPDM Propulsion System into orbit and use a high-power S-band radio to enable real-time operations in low Earth orbit (LEO) via the NASA Tracking and Data Relay Satellite System (TDRSS). The mission is working towards a tentative launch readiness date of August 2025, in support of launch and operations commencing in January 2026. This paper describes GPDM’s overall mission concept of operations, spacecraft overview, and subsystem breakdown.

Green Propulsion Dual Mode↗
NASA NTRS2002

HPLC/ESI-quadrupole ion trap mass spectrometry for characterization and direct quantification of amphoteric and nonionic surfactants in aqueous samples

An amphoteric (cocamidopropylbetaine, CAPB) and a nonionic (alcohol polyethoxylate, AE) surfactant were characterized by electrospray ionization quadrupole ion trap mass spectrometry (ESI-MS) as to their homologue distribution and ionization/fragmentation chemistry. Quantitative methods involving reversed-phase gradient HPLC and (+)ESI-MSn were developed to directly determine these surfactants in hydroponic plant growth medium that received simulated graywater. The predominant homologues, 12 C alkyl CAPB and 9 EO AE, were monitored to represent the total amount of the respective surfactants. The methods demonstrated dynamic linear ranges of 0.5-250 ng (r2 > 0.996) for CAPB and 8-560 ng (r2 > 0.998) for AE homologue mixture, corresponding to minimum quantification limits of 25 ppb CAPB and 0.4 ppm AE with 20-microL injections. This translated into an even lower limit for individual components due to the polydispersive nature of the surfactants. The procedure was successfully employed for the assessment of CAPB and AE biodegradation in a hydroponic plant growth system used as a graywater bioreactor.

NASA Discipline Life Support Systems↗
NASA NTRS1993

Secondary atomization in the combustion of electrostatic sprays

The combustion of electrosprays in a laminar counterflow diffusion flame has been experimentally studied by measuring droplet size and velocity distributions and gas-phase temperature. Detailed examination of the evolution of droplet size distribution as droplets approach the flame shows that, if substantial evaporation occurs before droplets 'interact' with the flame, the size distribution becomes bimodal. A secondary, sharp peak, in fact, develops in correspondence of diameters about one order of magnitude smaller than the mean. No evaporation mechanism can account for the development of such bimodality, that can be explained only in terms of a disintegration of droplets into finer fragments of size much smaller than the parent ones. This fission is of electric nature and it occurs when the repulsion of electric charges overcomes the surface tension cohesive force ultimately leading to a disintegration into finer fragments at or about the so-called Rayleigh limit. We here report on the first observation in combustion environments of such 'explosions'. If, on the other hand, droplets enter the very high temperature region before exploding, there appears to be no evidence of bimodality in their size distribution. In this case, in fact, flame chemi-ions may neutralize the charge on the droplets and thus prevent disruption.

Gomez, Alessandro↗
NASA NTRS1995

Proton affinity determinations and proton-bound dimer structure indications in C2 to C15, (alpha),(omega)-alkyldiamines

The 'kinetic method' was used to determine the proton affinity (PA) of a,coalkyldiamines from collision induced dissociation (CID) studies of protonated heterodimers. These PA values were consistently lower than those reported in the proton affinity scale. The apparent discrepancy was rationalized in terms of differences in the conformation of the protonated diamine monomers. The minimum energy species, formed by equilibrium proton transfer processes, have a cyclic conformation and the ion charge is shared by both amino-groups which are bridged by the proton. On the other hand, the species formed through dissociation of protonated dimers have a linear structure and the charge is localized on one of the amino-groups. Thus, the difference in the PA values obtained by both methods is a measure of the additional stability acquired by the protonated diamines through cyclization and charge delocalization. The major collision dissociation pathway of the protonated diamine monomers involved elimination of an ammonia moiety. Other reactions observed included loss of the second amino-group and several other bond cleavages. CID of the protonated dimers involved primarily formation of a protonated monomer through cleavage of the weaker hydrogen bond and subsequently loss of ammonia at higher collision energies. As observed from the CID studies, doubly charged ions were also formed from the diamines under conditions of the electrospray ionization.

Karpas, Z.↗
NASA NTRS2004

Lunar and Planetary Science XXXV: Astrobiology

The presentations in this session are: 1. A Prototype Life Detection Chip 2. The Geology of Atlantis Basin, Mars, and Its Astrobiological Interest 3. Collecting Bacteria Together with Aerosols in the Martian Atmosphere by the FOELDIX Experimental Instrument Developed with a Nutrient Detector Pattern: Model Measurements of Effectivity 4. 2D and 3D X-ray Imaging of Microorganisms in Meteorites Using Complexity Analysis to Distinguish Field Images of Stromatoloids from Surrounding Rock Matrix in 3.45 Ga Strelley Pool Chert, Western Australia 4. Characterization of Two Isolates from Andean Lakes in Bolivia Short Time Scale Evolution of Microbiolites in Rapidly Receding Altiplanic Lakes: Learning How to Recognize Changing Signatures of Life 5. The Effect of Salts on Electrospray Ionization of Amino Acids in the Negative Mode 6. Determination of Aromatic Ring Number Using Multi-Channel Deep UV Native Fluorescence 7. Microbial D/H Fractionation in Extraterrestrial Materials: Application to Micrometeorites and Mars 8. Carbon Isotope Characteristics of Spring-fed Iron-precipitating Microbial Mats 9. Amino Acid Survival Under Ambient Martian Surface UV Lighting Extraction of Organic Molecules from Terrestrial Material: Quantitative Yields from Heat and Water Extractions 10. Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods 11. Thermal Decomposition of Siderite-Pyrite Assemblages: Implications for Sulfide Mineralogy in Martian Meteorite ALH84001 Carbonate Globules 12. Determination of the Three-Dimensional Morphology of ALH84001 and Biogenic MV-1 Magnetite: Comparison of Results from Electron Tomography and Classical Transmission Electron Microscopy 13. On the Possibility of a Crypto-Biotic Crust on Mars Based on Northern and Southern Ringed Polar Dune Spots 14. Comparative Planetology of the Terrestrial Inner Planets: Implications for Astrobiology 15. A Possible Europa Exobiology 16. A Possible Biogeochemical Model for Titan

Source record↗
NASA NTRS2004

Atomic Oxygen Durability Evaluation of a UV Curable Ceramer Protective Coating

The exposure of most silicones to atomic oxygen in low Earth orbit (LEO) results in the oxidative loss of methyl groups with a gradual conversion to oxides of silicon. Typically there is surface shrinkage of oxidized silicone protective coatings which leads to cracking of the partially oxidized brittle surface. Such cracks widen and branch crack with continued atomic oxygen exposure ultimately allowing atomic oxygen to reach any hydrocarbon polymers under the silicone coating. A need exists for a paintable silicone coating that is free from such surface cracking and can be effectively used for protection of polymers and composites in LEO. A new type of silicone based protective coating holding such potential was evaluated for atomic oxygen durability in an RF atomic oxygen plasma exposure facility. The coating consisted of a UV curable inorganic/organic hybrid coating, known as a ceramer, which was fabricated using a methyl substituted polysiloxane binder and nanophase silicon-oxo-clusters derived from sol-gel precursors. The polysiloxane was functionalized with a cycloaliphatic epoxide in order to be cured at ambient temperature via a cationic UV induced curing mechanism. Alkoxy silane groups were also grafted onto the polysiloxane chain, through hydrosilation, in order to form a network with the incorporated silicon-oxo-clusters. The prepared polymer was characterized by H-1 and Si-29 NMR, FT-IR, and electrospray ionization mass spectroscopy. The paper will present the results of atomic oxygen protection ability of thin ceramer coatings on Kapton H as evaluated over a range of atomic oxygen fluence levels.

Banks, Bruce A.↗
NASA NTRS2003

Water-soluble Organic Components in Aerosols Associated with Savanna Fires in Southern Africa: Identification, Evolution and Distribution

During the SAFARI 2000 field campaign, both smoke aerosols from savanna fires and haze aerosols in the boundary layer and in the free troposphere were collected from an aircraft in southern Africa. These aerosol samples were analyzed for their water-soluble chemical components, particularly the organic species. A novel technique, electrospray ionization-ion trap mass spectrometry, was used concurrently with an ion chromatography system to analyze for carbohydrate species. Seven carbohydrates, seven organic acids, five metallic elements, and three inorganic anions were identified and quantified. On the average, these 22 species comprised 36% and 27% of the total aerosol mass in haze and smoke aerosols, respectively. For the smoke aerosols, levoglucosan was the most abundant carbohydrate species, while gluconic acid was tentatively identified as the most abundant organic acid. The mass abundance and possible source of each class of identified species are discussed, along with their possible formation pathways. The combustion phase of a fire had an impact on the chemical composition of the emitted aerosols. Secondary formation of sulfate, nitrate, levoglucosan, and several organic acids occurred during the initial aging of smoke aerosols. It is likely that under certain conditions, some carbohydrate species in smoke aerosols, such as levoglucosan, were converted to organic acids during upward transport.

Gao, Song↗
NASA NTRS2004

LC/MS Method for the Determination of Stable Isotope Labeled Promethazine in Human Plasma

Promethazine (PMZ) is taken by astronauts orally (PO), intramuscularly (IM) or rectally (PR) for space motion sickness. LC/MS method was developed with off-line solid phase extraction to measure plasma concentrations of PMZ given as stable isotope-labeled (SIL) formulations by the three different routes of administration simultaneously. Samples (0.5ml) were loaded on to Waters Oasis HLB co-polymer cartridges and eluted with 1.0 mL methanol. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 6 min. Acetonitrile/ ammonium acetate (30 mM) in water (3:2, v/v), pH 5.6 plus or minus 0.1, was used as the mobile phase for separation. Concentrations of PMZ, PMZ-d4 and PMZ-d7 and chlorpromazine (internal standard) were determined using a Micromass ZMD single quadrupole mass spectrometer with Electrospray Ionization (ESI). ESI mass spectra were acquired in positive ion mode with selected ion monitoring of [M+ H]dot plus. The method is rapid, reproducible and the assay specific parameters are listed in a table. A novel, sensitive and specific method for the measurement of PMZ and SIL PMZ in human plasma is reported.

Zuwei, Wang↗
NASA NTRS2005

Characterization of colloid thruster beams

In this article we use retarding potential, time of flight, and a Faraday cup, to measure the energy and specific charge distributions of the electrospray particles as a function of the position within the beam, as well as beam profiles. This information is then used, together with a model of the beam, to calculate its spreading.

electric propulsion↗
NASA NTRS2007

Determination of Scopolamine in Human Saliva Using Solid Phase Extraction and LC/MS/MS

Purpose: Scopolamine is the preferred treatment for motion sickness during space flight because of its quick onset of action, short half-life and favorable side-effect profile. The dose administered depends on the mode of administration and usually ranges between 0.1 and 0.8 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids by using conventional HPLC methods. To measure scopolamine in saliva and thereby to evaluate the pharmacokinetics of scopolamine, we developed an LC/MS/MS method using off-line solid phase extraction. Method: Samples (0.5mL) were loaded onto Waters Oasis HLB co-polymer cartridges (10 mg, 1 mL) and eluted with 0.5 mL methanol without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 4 minutes. The mobile phase for separation was 90:10 (v/v) methanol: ammonium acetate (2 mM) in water, pH 5.0 +/- 0.1. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 yields 138.1 and internal standard (IS) hyoscyamine m/z = 290.2 yields 124.1. Results: The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at 1.7 and 3.2 min respectively. The linear range is 50-5000 pg/mL for scopolamine in saliva with correlation coefficients > 0.99 with a CV < 0.5 %. The intra-day and inter-day CVs are < 15 % for quality control samples with concentrations of 75, 300, 750 and 3000 pg/mL of scopolamine in human saliva. Conclusion: Solid phase extraction allows more rapid sample preparation and greater precision than liquid extraction. Furthermore, we increased the sensitivity and specificity by adjusting the LC mobile phase and using an MS/MS detector.

Wang, Zuwei↗
NASA NTRS2008

A Modified LC/MS/MS Method with Enhanced Sensitivity for the Determination of Scopolamine in Human Plasma

Intranasal scopolamine is a choice drug for the treatment of motion sickness during space flight because of its quick onset of action, short half-life and favorable sideeffects profile. The dose administered usually ranges between 0.1 and 0.4 mg. Such small doses make it difficult to detect concentrations of scopolamine in biological fluids using existing sensitive LC/MS/MS method, especially when the biological sample volumes are limited. To measure scopolamine in human plasma to facilitate pharmacokinetic evaluation of the drug, we developed a sensitive LC/MS/MS method using 96 well micro elution plates for solid phase extraction (SPE) of scopolamine in human plasma. Human plasma (100-250 micro L) were loaded onto Waters Oasis HLB 96 well micro elution plate and eluted with 50 L of organic solvent without evaporation and reconstitution. HPLC separation of the eluted sample was performed using an Agilent Zorbax SB-CN column (50 x 2.1 mm) at a flow rate of 0.2 mL/min for 3 minutes. The mobile phase for separation was 80:20 (v/v) methanol: ammonium acetate (30 mM) in water. Concentrations of scopolamine were determined using a Micromass Quattro Micro(TM) mass spectrometer with electrospray ionization (ESI). ESI mass spectra were acquired in positive ion mode with multiple reaction monitoring for the determination of scopolamine m/z = 304.2 right arrow 138.1 and internal standard hyoscyamine m/z = 290.2 right arrow 124.1. The method is rapid, reproducible, specific and has the following parameters: scopolamine and the IS are eluted at about 1.1 and 1.7 min respectively. The linear range is 25-10000 pg/mL for scopolamine in human plasma with correlation coefficients greater than 0.99 and CV less than 0.5%. The intra-day and inter-day CVs are less than 15% for quality control samples with concentrations of 75,300, and 750 pg/mL of scopolamine in human plasma. SPE using 96 well micro elution plates allows rapid sample preparation and enhanced sensitivity for the LC/MS/MS determination of scopolamine in a small volume of biological samples. The new method is also cost effective since it uses a small volume of organic solvents compared to the methods using SPE cartridges or regular 96 well SPE plates. This method can be successfully used for bioavailability and pharmacokinetic evaluations of scopolamine, especially when volumes of biological samples are limited. Further investigation to use automated SPE system with 96 well micro elution plates is planned.

Wang, Zuwei↗