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At least 19 records
All sourcesNASA NTRSDOE OSTI
NASA NTRS1995

Coral Pigments: Quantification Using HPLC and Detection by Remote Sensing

Widespread coral bleaching (loss of pigments of symbiotic dinoflagellates), and the corresponding decline in coral reef health worldwide, mandates the monitoring of coral pigmentation. Samples of the corals Porites compressa and P. lobata were collected from a healthy reef at Puako, Hawaii, and chlorophyll (chl) a, peridinin, and Beta-carotene (Beta-car) were quantified using reverse-phase high performance liquid chromatography (HPLC). Detailed procedures are presented for the extraction of the coral pigments in 90% acetone, and the separation, identification, and quantification of the major zooxanthellar pigments using spectrophotometry and a modification of the HPLC system described by Mantoura and Llewellyn (1983). Beta-apo-8-carotenal was found to be inadequate as in internal standard, due to coelution with chl b and/or chl a allomer in the sample extracts. Improvements are suggested, which may result in better resolution of the major pigments and greater accuracy in quantification. Average concentrations of peridinin, chl a, and Beta-car in corals on the reef were 5.01, 8.59, and 0.29, micro-grams/cm(exp 2), respectively. Average concentrations of peridinin and Beta-car did not differ significantly between the two coral species sampled; however, the mean chl a concentration in P. compressa specimens (7.81 ,micro-grams/cm(exp 2) was significantly lower than that in P. lobata specimens (9.96 11g/cm2). Chl a concentrations determined spectrophotometrically were significantly higher than those generated through HPLC, suggesting that spectrophotometry overestimates chl a concentrations. The average ratio of chl a-to-peridinin concentrations was 1.90, with a large (53%) coefficient of variation and a significant difference between the two species sampled. Additional data are needed before conclusions can be drawn regarding average pigment concentrations in healthy corals and the consistency of the chl a/peridinin ratio. The HPLC pigment concentration values contribute to the limited database of pigment concentrations in healthy corals, from which quantitative definitions of 'healthy' vs. 'bleached' coral may emerge. They also serve as ground-truth, corresponding to fluorescence data collected from the reef at Puako using airborne remote sensing of laser induced fluorescence. Fluorescence spectra from several overflights using the NASA AOL (airborne oceanographic lidar) system show consistent chlorphyll fluorescence peaks around 685 nm, as well as consistence peaks in the 400-600 nm range which may emanate from granules in the coral tissue. These data, along with results from previous studies of coral fluorescence, suggest that remote sensing of laser-induced fluorescence may become a rapid and efficient means of monitoring coral pigmentation and coral reef bleaching.

Cottone, Mary C.↗
NASA NTRS1979

HPLC for quality control of polyimides

High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

Young, P. R.↗
NASA NTRS1989

Improved method for HPLC analysis of polyamines, agmatine and aromatic monoamines in plant tissue

The high performance liquid chromatographic (HPLC) method of Flores and Galston (1982 Plant Physiol 69: 701) for the separation and quantitation of benzoylated polyamines in plant tissues has been widely adopted by other workers. However, due to previously unrecognized problems associated with the derivatization of agmatine, this important intermediate in plant polyamine metabolism cannot be quantitated using this method. Also, two polyamines, putrescine and diaminopropane, also are not well resolved using this method. A simple modification of the original HPLC procedure greatly improves the separation and quantitation of these amines, and further allows the simulation analysis of phenethylamine and tyramine, which are major monoamine constituents of tobacco and other plant tissues. We have used this modified HPLC method to characterize amine titers in suspension cultured carrot (Daucas carota L.) cells and tobacco (Nicotiana tabacum L.) leaf tissues.

Non-NASA Center↗
NASA NTRS2005

The Second SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-2)

Eight international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a variety of laboratory standards. The field samples were collected primarily from eutrophic waters, although mesotrophic waters were also sampled to create a dynamic range in chlorophyll concentration spanning approximately two orders of magnitude (0.3 25.8 mg m-3). The intercomparisons were used to establish the following: a) the uncertainties in quantitating individual pigments and higher-order variables (sums, ratios, and indices); b) an evaluation of spectrophotometric versus HPLC uncertainties in the determination of total chlorophyll a; and c) the reduction in uncertainties as a result of applying quality assurance (QA) procedures associated with extraction, separation, injection, degradation, detection, calibration, and reporting (particularly limits of detection and quantitation). In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied. The culmination of the activity was a validation of the round-robin methodology plus the development of the requirements for validating an individual HPLC method. The validation process includes the measurements required to initially demonstrate a pigment is validated, and the measurements that must be made during sample analysis to confirm a method remains validated. The so-called performance-based metrics developed here describe a set of thresholds for a variety of easily-measured parameters with a corresponding set of performance categories. The aggregate set of performance parameters and categories establish a) the overall performance capability of the method, and b) whether or not the capability is consistent with the required accuracy objectives.

Source record↗
NASA NTRS2011

An Investigation Into HPLC Data Quality Problems

This report summarizes the analyses and results produced by a five-member investigative team of Government, university, and industry experts, established by NASA HQ. The team examined data quality problems associated with high performance liquid chromatography (HPLC) analyses of pigment concentrations in seawater samples produced by the San Diego State University (SDSU) Center for Hydro-Optics and Remote Sensing (CHORS). This report shows CHORS did not validate the methods used before placing them into service to analyze field samples for NASA principal investigators (PIs), even though the HPLC literature contained easily accessible method validation procedures, and the importance of implementing them, more than a decade ago. In addition, there were so many sources of significant variance in the CHORS methodologies, that the HPLC system rarely operated within performance criteria capable of producing the requisite data quality. It is the recommendation of the investigative team to a) not correct the data, b) make all the data that was temporarily sequestered available for scientific use, and c) label the affected data with an appropriate warning, e.g., "These data are not validated and should not be used as the sole basis for a scientific result, conclusion, or hypothesis--independent corroborating evidence is required."

Hooker, Stanford B.↗
NASA NTRS1986

A thin film degradation study of a fluorinated polyether liquid lubricant using an HPLC method

A High Pressure Liquid Chromatography (HPLC) separation method was developed to study and analyze a fluorinated polyether fluid which is promising liquid lubricant for future applications. This HPLC separation method was used in a preliminary study investigating the catalytic effect of various metal, metal alloy, and ceramic engineering materials on the degradation of this fluid in a dry air atmosphere at 345 C. Using a 440 C stainless steel as a reference catalytic material it was found that a titanium alloy and a chromium plated material degraded the fluorinated polyether fluid substantially more than the reference material.

Morales, W.↗
NASA NTRS2010

The Fourth SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-4)

Ten international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a mixed pigment sample. Although prior Sea-viewing Wide Field-of-view Sensor (SeaWiFS) High Performance Liquid Chromatography (HPLC) Round-Robin Experiment (SeaHARRE) activities conducted in open-ocean waters covered a wide dynamic range in productivity, and some of the samples were collected in the coastal zone, none of the activities involved exclusively coastal samples. Consequently, SeaHARRE-4 was organized and executed as a strictly coastal activity and the field samples were collected from primarily eutrophic waters within the coastal zone of Denmark. The more restrictive perspective limited the dynamic range in chlorophyll concentration to approximately one and a half orders of magnitude (previous activities covered more than two orders of magnitude). The method intercomparisons were used for the following objectives: a) estimate the uncertainties in quantitating individual pigments and higher-order variables formed from sums and ratios; b) confirm if the chlorophyll a accuracy requirements for ocean color validation activities (approximately 25%, although 15% would allow for algorithm refinement) can be met in coastal waters; c) establish the reduction in uncertainties as a result of applying QA procedures; d) show the importance of establishing a properly defined referencing system in the computation of uncertainties; e) quantify the analytical benefits of performance metrics, and f) demonstrate the utility of a laboratory mix in understanding method performance. In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied.

Hooker, Stanford B.↗
NASA NTRS1987

Quantitative analysis of PMR-15 polyimide resin by HPLC

The concentration of individual components and of total solids of 50 wt pct PMR-15 resin solutions was determined using reverse-phase HPLC to within + or - 8 percent accuracy. Acid impurities, the major source of impurities in 3,3', 4,4'-benzophenonetetracarboxylic acid (BTDE), were eliminated by recrystallizing the BTDE prior to esterification. Triester formation was not a problem because of the high rate of esterification of the anhydride relative to that of the carboxylic acid. Aging of PMR-15 resin solutions resulted in gradual formation of the mononadimide and bisnadimide of 4,4'-methylenedianiline, with the BTDE concentration remaining constant. Similar chemical reactions occurred at a reduced rate in dried films of PMR-15 resin.

Roberts, Gary D.↗
NASA NTRS2001

The First SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-1)

Four laboratories, which had contributed to various aspects of SeaWiFS calibration and validation activities, participated in the first SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-1): Horn Point Laboratory (USA), the Joint Research Centre (Italy), the Laboratoire de Physique et Chimie Marines (France), and the Marine and Coastal Management group (South Africa). The analyses of the data are presented in Chapter 1 and the individual methods of the four groups are presented in Chapters 2-5. The average (or overall) conclusions of the round-robin are derived from 12 in situ stations occupied during a cruise in the Mediterranean Sea, although, only 11 stations are used in the analyses. The data set is composed of 12 replicates taken during each sampling opportunity with 3 replicates going to each of the 4 laboratories. The average (or overall) results from the intercomparison of 15 pigments or pigment associations are as follows (in some cases, data subsets that exclude pigments which were not analyzed by all the laboratories, or that had unusually large variances, are used to exclude a variety of problematic pigments): a) the accuracy of the four methods in determining the concentration of total chlorophyll a is 7.9%, (one method did not separate mono- and divinyl chlorophyll a, and if the samples containing significant divinyl chlorophyll a concentrations are ignored, the four methods have an accuracy of 6.7%); b) the accuracy in determining the full set of pigments is 19.1%; c) there is a reduction in accuracy of approximately - 12.2% for every decade (factor of 10) decrease in concentration (based on a data subset); d) the precision of the four methods using a subset data is 8.617( 6.2% for an edited subset); e) the repeatability of the four methods using the subset data is 9.2% (7.2%; for an edited subset, and f) the reproducibility of the four methods using the subset data is 21.31% (15.0% for an edited subset).

Hooker, Stanford B.↗
NASA NTRS2004

Laboratory Detection and Analysis of Organic Compounds in Rocks Using HPLC and XRD Methods

In this work we describe an analytical method for determining the presence of organic compounds in rocks, limestone, and other composite materials. Our preliminary laboratory experiments on different rocks/limestone show that the organic component in mineralogical matrices is a minor phase on order of hundreds of ppm and can be better detected using high precision liquid chromatography (HPLC). The matrix, which is the major phase, plays an important role in embedding and protecting the organic molecules from the harsh Martian environment. Some rocks bear significant amounts of amino acids therefore, it is possible to identify these phases using powder x-ray diffraction (XRD) by crystallizing the organic. The method of detection/analysis of organics, in particular amino acids, that have been associated with life will be shown in the next section.

Dragoi, D.↗
NASA NTRS2000

Correlation of lycopene measured by HPLC with the L, a, b color readings of a hydroponic tomato and the relationship of maturity with color and lycopene content

Tomatoes (Lycopersicon esculentum cv. Laura) were separated, according to the ripening stage, by a sensory panel into seven groups, and color was measured on the tomato surface with a Minolta Chroma meter. The L, a, b, hue, chroma, and lycopene content were plotted against the maturity stages of the tomatoes, and several good correlations were found. The a/b ratio and the lycopene content were the parameters that allowed six of seven maturity groups in the tomato to be statistically distinguished. The lycopene content, measured by HPLC, was also correlated with the color measurements, and the a, a/b, and (a/b)(2) color factors produced the best regressions. An estimation of the lycopene content in tomatoes can be achieved by using a portable chroma meter, with a possible field usage application. Equations to calculate the lycopene content of tomatoes based on the color readings are reported.

Non-NASA Center↗
NASA NTRS2009

The Third SeaWiFS HPLC Analysis Round-Robin Experiment (SeaHARRE-3)

Seven international laboratories specializing in the determination of marine pigment concentrations using high performance liquid chromatography (HPLC) were intercompared using in situ samples and a mixed pigment sample. The field samples were collected primarily from oligotrophic waters, although mesotrophic and eutrophic waters were also sampled to create a dynamic range in chlorophyll concentration spanning approximately two orders of magnitude (0.020 1.366 mg m^{-3}) The intercomparisons were used to establish the following: a) the uncertainties in quantitating individual pigments and higher-order variables (sums, ratios, and indices); b) the reduction in uncertainties as a result of applying quality assurance (QA) procedures; c) the importance of establishing a properly defined referencing system in the computation of uncertainties; d) the analytical benefits of performance metrics, and e) the utility of a laboratory mix in understanding method performance. In addition, the remote sensing requirements for the in situ determination of total chlorophyll a were investigated to determine whether or not the average uncertainty for this measurement is being satisfied.

Hooker, Stanford B.↗
NASA NTRS2020

Precision Assessment of the HPLC Phytoplankton Pigment Dataset Analyzed by NASA to Quantify Global Variability in Support of Ocean Color Remote Sensing

The ability to generate chlorophyll a (Chl a) assessments from ocean color orbital sensors, such as VIIRS and MODIS, that satisfy the requirements to be climate-quality data record (CDR) quality is contingent in part on the quality of the in situ ground or sea truth observations that serve as datasets for vicarious calibration and algorithm validation activities. NASA has a mandate to collect, analyze, and distribute in situ data of the highest possible quality with documented uncertainties and in keeping with established performance metrics. Using a dataset of over 18,000 HPLC phytoplankton pigment samples representing water collected in all major ocean basins analyzed a central laboratory (Field Support Group (FSG) of the Ocean Ecology Laboratory (OEL) at NASA Goddard Space Flight Center (GSFC)), we performed an assessment of the global precision among sample replicates of Chl a as well as major accessory pigments. We investigated the impacts of filtration volume, water basin, collection technique, pigment concentration, and different filtration volumes for replicate filters on replicate filter precision, as well as investigating any pigment-specific differences. Our results quantify sample variability with the goal of understanding any systemic biases or biogeographic influences.

Thomas, Crystal S.↗
NASA NTRS1985

Direct coupling of microbore HPLC columns to MS systems

A detailed investigation using electron microscopy was conducted which examined the conditions of materials used in the construction of stable, high performance microbore liquid chromatography (LC) columns. Small details proved to be important. The effects of temperature on the elution of several homologous series used as probe compounds was examined in reverse phase systems. They showed that accessible temperature changes provide roughly half the increase in solvent strength that would be obtained going from a 100% aqueous to a 100% organic mobile phase, which is sufficient to warrant their use in many analyses requiring the use of gradients. Air circulation temperature control systems provide the easiest means of obtaining rapid, wide range changes in column temperature. However, slow heat transfer from the gas leads to thermal nonuniformity in the column and a decrease in resolution as the temperature program progresses.

Mcnair, H. M.↗
NASA NTRS1999

HPLC Characterization of Phenol-Formaldehyde Resole Resin Used in Fabrication of Shuttle Booster Nozzles

A reverse phase High Performance Liquid Chromatographic method was developed to rapidly fingerprint a phenol-formaldehyde resole resin similar to Durite(R) SC-1008. This resin is used in the fabrication of carbon-carbon composite materials from which Space Shuttle Solid Rocket Booster nozzles are manufactured. A knowledge of resin chemistry is essential to successful composite processing and performance. The results indicate that a high quality separation of over 35 peaks in 25 minutes were obtained using a 15 cm Phenomenex LUNA C8 bonded reverse phase column, a three-way water-acetonitrile-methanol nonlinear gradient, and LTV detection at 280 nm.

Young, Philip R.↗
NASA NTRS1987

Comparison of automated pre-column and post-column analysis of amino acid oligomers

It has been shown that various amino acids will polymerize under plausible prebiotic conditions on mineral surfaces, such as clays and soluble salts, to form varying amounts of oligomers (n = 2-6). The investigations of these surface reactions required a quantitative method for the separation and detection of these amino acid oligomers at the picomole level in the presence of nanomole levels of the parent amino acid. In initial high-performance liquid chromatography (HPLC) studies using a classical postcolumn o-phthalaldehyde (OPA) derivatization ion-exchange HPLC procedure with fluorescence detection, problems encountered included lengthy analysis time, inadequate separation and large relative differences in sensitivity for the separated species, expressed as a variable fluorescent yield, which contributed to poor quantitation. We have compared a simple, automated, pre-column OPA derivatization and reversed-phase HPLC method with the classical post-column OPA derivatization and ion-exchange HPLC procedure. A comparison of UV and fluorescent detection of the amino acid oligomers is also presented. The conclusion reached is that the pre-column OPA derivatization, reversed-phase HPLC and UV detection produces enhanced separation, improved sensitivity and faster analysis than post-column OPA derivatization, ion-exchange HPLC and fluorescence detection.

NASA Discipline Exobiology↗