bluuebunny/crossref_metadata_2025_split huggingface dataset:
Investigation of the steady state measurement process
Authors: Nagy J. L. , Leisztner L. , Hangos K. M. 
Published: March 2007

Based on the role of steady state concept in the model of analytical chemical measurement and deduction, the definition of ‘practically sleady slate’ (PSS) has been inlroduced. The defnition does not require the process to be in steady state in a strictly mathematical sense. In order to fulfil the requiremenls of ‘practically steady state’ the random error and the syslematic error must vary within a suitable limit, and the expected fgure for the measured value must be within a specified range.The goal of the present investigation was to detect the steady state of the measurement process with respect to the analytical information (peak area ratio) based on the measured values. The method proposed proved to be useful for the determination of the simultaneously present systematic error and random error. Control based on the measured values of the internal standard is useful, but additional information is necessary. There are several advantages to the method described: the results for the internal standard indicate possible sources of disturbances and allow the end of the steady state measurement process to be predicted.
An evaluation of the Diamat HPLC analyserfor simultaneous determination ofhaemoglobins A2 and F
Authors: Mosca Andrea , Carpinelli Assunta , Majavacca Rita , Cantu′-Rajnoldi Angelo , Garatti Massimo , Paleari Renata , Ferrari Maurizio , Agape Vittorio , Maccioni Liliana , Pisano Sandra , Galanello Renzo 
Published: March 2007

The authors describe a modification of the instrumental parameters
of the Diamat fully automated HPLC system for Hb A2 assay
(Bio‐Rad Laboratories, Milan, Italy) in order to obtain
simultaneous determination of Hb A2 and Hb F.Hb A2 and Hb F measurements are reproducible (within‐run CV
2.6%, with Hb A22.7%; 5.1%, with Hb F 1.3%) and accurate
(from a comparison with two microchromatographic techniques for
Hb A2: r = 0.9639 and 0.9755; with two alkali denaturation
procedures for Hb F: r = 0.9990 and 0.9952; with radial
immunodiffusion, r = 0.9877). Assay linearity has been confirmed
for Hb A2 concentrations between 0 and 6.0%, and for Hb F
between 0 and 60%. The data obtained from the analysis of some
pathological samples for Hb Bart′s, Hb H, Hb J Sardegna, Hb
Lepore and Hb S are in agreement with cellulose acetate
electrophoresis analysis.The Hb A2 reference intervals for normals (N = 597) and
Beta‐thalassemia carriers (N = 200) are respectively (95%
limits) 2.02‐3.27 and 3.92‐5.90 in % units. Hb F values
measured in normals (N = 968), in β‐thal carriers (N = 302) and
in δβ‐thal carriers (N =3) have been found to be consistent with
the usual diagnostic parameters.Some minor limitations emerged: the most relevant concerns Hb
A1c, which is overestimated with respect to a reference method (y =
1.217x + 0.16; N = 79; r = 0.9235). A probable interference
from labile fractions is responsible for this Hb A1c inaccuracy.
Evaluation of the Jokoo‐ION 150 AC: Guidelines for the evaluation of analysers by ion‐selective electrodes
Authors: Farré Joan , Biosca Carmen , Galimany Román 
Published: March 2007

The Jokoo‐ION 150 AC is an automatic sodium, potassium and chloride analyser which uses ion‐selective electrodes.The sample mode can be whole‐blood, serum or urine. To evaluate a urine sample, a previous dilution (1:6) with the standard 1 solution is required. For three concentrations of control materials, the total precision (CV) ranged from 0.17 to 1.22% for sodium, 0.22 to 1.69% for potassium and 0.16 to 0.74% for chloride.The system demonstrated acceptable performance in detection limit, linearity, drift and carry‐over. Patients′ results from ION 150 AC correlated well with those from a SMAC II and an IL 943. In a study on potential interferences, a slightly negative interference with potassium was found with increases in lithium; and only high ammonium ion concentrations caused a positive interference on the potassium ion. A slightly positive interference of bromide on the chloride ion was also found.The electrode slope, electrode response, sample temperature and pH effect, effects of high concentrations of proteins or lipids, and haematocrit influence on the sodium, potassium and chloride ion concentration were also evaluated. The strategy adopted in this study provides an ideal framework for future evaluations of ionselective electrode analysers.
Evaluation of the Dacos 3.0 analyser
Authors: Pons Joan Farré , Alumá Alba , Antoja Felipe , Biosca Carmen , Alsina María-Jesús , Galimany Román 
Published: March 2007

The selective multitest Coulter Dacos 3.0 analyser was evaluated according to the guidelines of the Comisión de Instrumentación de la Sociedad Española de Química Clínica and of the European Committee for Clinical Laboratory Standards.The evaluation was performed in four steps: examination of the analytical units; evaluation of routine working; study of interferences; and assessment of practicability.The evaluation included a photometric study. The inaccuracy is acceptable for 340 nm and 420 nm, and the imprecision at absorbances from 0.05 to 2.00 ranged from 0.06 to 0.28% at 340 nm and from 0.06 to 0.08% at 420 nm. The linearity showed some dispersion at low absorbance for PNP at 420 nm and the drift was negligible.The imprecision of the pipette delivery system, the temperature control system and the washing system were satisfactory.In routine work conditions, seven analytical methods were studied: glucose, creatinine, iron, total protein, AST, ALP and calcium. Within‐run imprecision ranged, at low concentrations, from 0.9% (CV) for glucose, to 7.6% (CV) for iron; at medium concentrations, from 0.7% (CV) for total protein to 5.2% (CV) to creatinine; and at high concentrations, it ranged from 0.6% (CV) for glucose to 3.9% (CV) for ALP.Between‐run imprecision at low concentrations ranged from 1.4% (CV) for glucose to 15.1% (CV) for iron; at medium concentrations it ranged from 1.2% (CV) for protein to 6.7% (CV) for iron; and at high concentrations the range is from l.2for AST to 5.7% (CV) for iron.No contamination was found in the sample carry‐over study. Some contamination was found in the reagent carry‐over study (total protein due to iron and calcium reagents). Relative inaccuracy is good for all the constituents assayed. Only LDH (high and low levels) and urate (low level) showed weak and negative interference caused by turbidity, and γ‐GT (high level) and amylase, bilirubin and ALP (two levels) showed a negative interference caused by haemolysis.
Comparison of capillary gas chromatographic method and automatedspectrophotofluorometric methods for measuring content uniformity of conjugatedoestrogens in pharmaceutical preparations
Authors: Russell J. D. , Mumley J. , Spring M. , Kutz A. , Johnson R. N. 
Published: March 2007

To measure the content uniformity of conjugated cestrogens tablets,
the USP XXII monograph specifies a capillary gas chromatographic method. This involves separation of the trimethylsilyl derivatives of the various oestrogens found in a typical conjugated oestrogens tablet using a fused‐silica 0V 225 bonded phase column. Hydrogen is used as the carrier gas with FID detection. A more rapid spectrophotofluorometric method of analysis has been developed in which the oestrogens are extracted from the dosage form into water, then transferred into organic solvent as the dicyclohexylamine complex. Fluorescence is developed by heating the solution of the complex in the presence of 70% sulphuric acid. The chemistry and detection are carried out using a segmented‐flow analyser.The spectrophotofluorometric method is preferred as a routine control for content uniformity because considerable time is saved during sample preparation and analysis compared to gas chromatography. Coefficients of variation show that both methods produce
acceptable results. These results fall well within the USP XXII [1] monograph, limits and also well within the tighter limits imposed by the USP XXII, section 905.
Designing optimized industrial process analysers for closed loop control
Authors: Grevesmuehl Bernard , Kradjel Cynthia , Kellner Hanno 
Published: March 2007

Manufacturers are now looking closely at ways of optimizing
‘quality’ and increasing process efficiency while reducing manufacturing
costs. Near infra‐red (NIR) technology is a popular solution to this challenge: it provides manufacturers with rapid and reliable in‐process analysis and thousands of systems have already been installed in the food, chemical, pharmaceutical and agricultural markets.For over 10 years, NIR has been successfully applied to at‐line process analysis. Rugged and easy‐to‐operate filter analysers are traditionally located in the control room–process operators can then ‘grab samples’ and obtain results in less than a minute. There are many practical advantages to using at‐line filter systems.
Products from many lines can be run on one system, and, since there is no direct process interface, installation, operation and maintenance are quite simple.Many manufacturers, however, are now striving to achieve on‐line closed loop control, in these cases the benefit of obtaining continuous measurement is well worth the effort required to automate the analysis.
Automation of Vapour Pressure Osmometry measurements
Authors: Belaustegi Y. , Citores M. J. , Fernández L. A. 
Published: March 2007

A program has been developed for the control of Vapour Pressure
Osmometry (VPO) measurements. The output signal of a Vapour Pressure Osmometer is read by an A/D converter card installed in one of the expansion slots of a PC microcomputer. The stability of the measurements is checked by analysing the first derivative of the smoothed signals, which is calculated in real time. Sets of repeated
measurements are carried out under the supervision of a computer program as a check for their reproducibility. When the set is ended the program calculates the average and its standard deviation.The program is particularly valuable for evaluating VPO measurements for solution equilibria studies. This interfacing strategy may be applied to any kind of technique in which the time stability of the signals is the basis for defining measurement stability. The automated VPO has other advantages, including low cost and time saving.
Evaluation of the Olympus AU‐510 analyser
Authors: Farré Carmen , Velasco Jesús , Ramón Francisco 
Published: March 2007

The selective multitest Olympus AU‐510 analyser was evaluated
according to the recommendations of the Comision de Instrumentacion de la Sociedad Española de Quimica Clinica and the European Committee for Clinical Laboratory Standards. The evaluation was carried out in two stages: an examination of the analytical units and then an evaluation in routine work conditions. The operational characteristics of the system were also studied.The first stage included a photometric study: dependent on the absorbance, the inaccuracy varies between +0.5% to ‐0.6% at 405 nm and from ‐5.6% to 10.6% at 340 nm; the imprecision ranges between ‐0.22% and 0.56% at 405 nm and between 0.09% and 2.74% at 340 nm. Linearity was acceptable, apart
from a very low absorbance for NADH at 340 nm; and the imprecision of the serum sample pipetter was satisfactory.Twelve serum analytes were studied under routine conditions: glucose, urea urate, cholesterol, triglycerides, total bilirubin, creatinine, phosphate, iron, aspartate aminotransferase, alanine aminotransferase and gamma‐glutamyl transferase.The within‐run imprecision (CV%) ranged from 0.67% for phosphate to 2.89% for iron and the between‐run imprecision from 0.97% for total bilirubin to 7.06% for iron. There was no carryover in a study of the serum sample pipetter. Carry‐over studies with the reagent and sample pipetters shows some cross contamination in the iron assay.
Technical note: A nonparametric outlier rejection scheme
Authors: Odonde J. S. O. 
Published: March 2007

Experimental data always contains measurement errors (or noise,
in signal processing). This paper is concerned with the removal of
outliers from a data set consisting of only a handful of points. The
data set has a unimodal probability distribution function, the mode
is thus a reliable estimate of the central tendency. The approach is
nonparametric; for the data set (xi, yi) only the ordinates (yi) are
used. The abscissa (xi) are reparametrized to the variable i = 1, N.The data is bounded using a calculated mode and a new measure:
the mean absolute deviation from the mode. This does not seem to
have been reported before. The mean is removed and low frequency
filtering is performed in the frequency domain, after which the mean
is reintroduced.
The laboratory of the 1990s—Planning for Total Automation
Authors: Brunner Linda A. 
Published: March 2007

The analytical laboratory of the 1990s must be able to meet and
accommodate the rapid evolution of modern‐day technology. One
such area is laboratory automation. Total automation may be seen
as the coupling of computerized sample tracking, electronic
documentation and data reduction with automated sample handling,
preparation and analysis, resulting in a complete analytical
procedure with minimal human involvement. Requirements may
vary from one laboratory or facility to another, so the automation
has to be flexible enough to cover a wide range of applications, and
yet fit into specific niches depending on individual needs.Total automation must be planned for, well in advance, if the
endeavour is to be a success. Space, laboratory layout, proper
equipment, and the availability and access to necessary utilities
must be taken into account. Adequate training and experience of the
personnel working with the technology must also be ensured. In
addition, responsibilities of installation, programming maintenance
and operation have to be addressed. Proper time management
and the efficient implementation and use of total automation are
also crucial to successful operations.This paper provides insights into laboratory organization and
requirements, as well as discussing the management issues that
must be faced when automating laboratory procedures.
Selection criteria for laboratory roboticapplication personnel
Authors: Rulon Peter W. 
Published: March 2007

Norwich Eaton Pharmaceutical recognized the benefits of using
automation systems in the laboratory over seven years ago and
created a robotic development area within the analytical method
development group. They now have eight complete robotic systems
and a large number of semi‐automated systems in routine operation.This level of activity has provided many challenges for the
automation group. The success of this group has been very dependent
on the talents of people working these assignments. You can have the
best equipment and the vendor′s promises of success, but it is the
people who understand the products and the requirements that get
systems on line.Assembling an effective robotics organization requires prework on
the part of management. There must be a clear vision of the specific
types of activities the group will perform. This vision can be used to
establish a skills profile for the members of the team. It appears that
at least four people are required to provide the variety of skills and
keep the group going.Each member′s personality is an important component of
establishing a new team. In robotics, one of the most critical talents
is the ability to work on long term projects that constantly present
new challenges. The group members need to balance consistency of
purpose with the ability to creatively solve a variety of problems.
The group will not be effective in delivering new technologies unless
they have the talent to train the novice in a highly technical
environment.People who are successful in automation development are unique.
They should have the ability to work comfortably in a logic‐based
environment, to become very creative on demand, and to communicate
highly technical information effectively. People do not usually
possess all these skills, providing their manager with challenging
coaching opportunities.
Application of a computer‐controlled flow analyser to the determination of glucose andto the study of β ‐galactosidase activity
Authors: Malcolme-Lawes David J. , Wong Koon Hung , Smith Brian V. 
Published: March 2007

Glucose was determined using an automated flow analyser and a commercial reagent preparation based on the glucose oxidaseperoxidase reaction. The coupling system for the hydrogen peroxide
liberated consisted of 4‐aminophenazone and 2,4‐dichlorophenol. The analyser demonstrated linearity of>0.9997 for five consecutive sets of standards. The average RSD for individual standards is
0.76%, and a sample throughput rate of >80 h-1 was achieved.The study of β‐galactosidase, using a novel substrate, was carried out in a simple single‐line manifold. The enzyme‐substrate reaction mixture was injected into a pH 10 buffer carrier to stop the reaction, and at the same time, propel the reaction zone to the flow cell. Km and Vmax values were calculated.
Plasma amino‐acid determinations by reversed‐phase HPLC: Improvement of theorthophthalaldehyde method and comparison with ion exchange chromatography
Authors: Ziegler Frédéric , Le Boucher Jacques , Coudray-Lucas Colette , Cynober Luc 
Published: March 2007

Reversed‐phase high performance liquid chromatographic (RPHPLC)
determination of amino‐acids with on‐line pre‐column
ortho‐phthalaldehyde (OPA) derivatization and fluorescence
detection is rapid and sensitive. However, high‐performance ionexchange
chromatography (HP‐IEC) with post‐column ninhydrine
reaction is the most widely used amino‐acid (AA) assay for
biological samples. These two methods have been compared for the
determination of individual plasma AA concentrations.An excellent correlation (p ≤ 0.003) was found between the results
given by an RP‐HPLC system (Varian) and a classical AA autoanalyser
(Biotronik LC 5001). Most AA concentrations were
similar with the two methods, but a paired t‐test showed slight
differences for 13 AA. The within‐batch reproducibility of the RPHPLC
method was comparable to that of the HP‐IEC method.
The analysis was about three times faster with RP‐HPLC, and
sensitivity was l00‐fold better. However, aspartic acid, proline and
cysteine were not identified by the RP‐HPLC method, while the
tryptophan quantification is possible.RP‐HPLC with automated pre‐column OPA derivatization is
clearly a suitable alternative for assaying physiological AA and
may be particularly useful for AA present at low concentrations
(free tryptophan, plasma 3‐methylhistidine).
Automated sampling and analysis inresearch product synthesis
Authors: Timmermans L. , den Bergh A. Van , Verhecken A. , de Sande C. Van 
Published: March 2007

The information obtained about relevant reaction parameters can be
greatly increased by monitoring concentration changes during a
reaction. To achieve this goal, a fully automated system was
designed which handles both sampling and analysis. The sampling
system takes samples at predefined intervals, and also performs a
number of tasks such as dilution, neutralization, filtration and
analysis.The examples show the universal applicability of the device
regarding to solvents, reaction media and reaction type. It is also
demonstrated that the information, included in the concentration
profiles, greatly increases our knowledge about the reaction. This
increase in information, in conjunction with other data,for example
calorimetry, could be used for reaction simulation software.
Analytical performance of the selective multianalyser Olympus AU 5200
Authors: Mayer H. , Luley C. , Behnke M. , Wieland H. 
Published: March 2007

The analytical performance of a selective, automatic multianalyser‐ the Olympus A U5200 ‐ was tested and assessed for practicability, following ECCLSguidelines. Twenty‐two analytes were tested and compared with the Olympus A U5000 analyser. A Hitachi 747 analyser was also included in this survey in order to obtain correlation data for ISE measurements.The imprecision data, expressed as median CV values, were found to be below 2% in series for 21 parameters, and below 3% for 19 paramaters from day to day. Creatinine measured with the kinetic Jaffe method obtained a median CV value of 4% in series, creatine phosphokinase showed the worst imprecision from day to day with a CV of 9%. Slightly better precision values for the majority ofall tests were found on the Olympus AU5200 than on the AU 5000 analyser.The recovery of the assigned values in 32 commercial control sera was between 95% and 105% for 14 tests. Five of the remaining tests yielded recoveries with deviations between 5% and 10%, deviations above 10% showed albumine, alanine aminotransferase, aspartate aminotransferase and creatine phosphokinase. The accuracy of most test parameters was slightly better on the AU5200 analyser than on the comparison instrument.The range of linearity ofthe tested methods covered the range stated by the manufacturers; and no sample carry‐over was detected. Most parameters tested yielded close correlation to those on the comparison instrument. Amylase measurements on both analysers correlate well but are not comparable without data correction due to different test methods. In addition, no drift effects were observed over a period of 9 hours.The ion‐selective‐electrode unit performed well in terms of throughput, precision and stability over time. The whole system showed good practicability with respect to patient sample and reagent handling, a short training period of technicians, ease of system software, maintenence, a robust barcode reader and a flexible host communication procedure.
Fully‐automated system for dissolution rate of solid oral dosage forms according to the paddle method
Authors: Lamparter Erich , Riedl Dieter 
Published: March 2007

This paper describes a fully‐automated system (AUTO DISS®) for the determination of active ingredient release of solid oral dosage forms according to the paddle method of the US Pharmacopoeia (USP) and European Pharmacopoeia.Twenty batches can be tested continuously, with the six individuals (tablets, capsules etc.) of one batch being examined synchronous. The components of the AUTO DISS® system are presented and the operating steps of automatic filling with dissolution medium, dropping in of tablets, sampling and cleaning of vessels are described. Suitability for testing controlled‐release drugs by means of automated buffer change from simulated gastric fluid to simulated intestinal fluid according to USP is also demonstrated. On‐line determination of active ingredient concentration, as well as evaluation and documentation of measured values, is possible using an integrated automatic sampler in combination with various measuring instruments.The AUTO DISS® system is shown to be both rugged and accurate.