Automated method using

Amador, E. Salvatore, A. C. Serum gluatmic-oxalacetic transaminase activity. Revised manual and automated methods using diazonium dyes. Am. J. Clin. Path. (1971), 55, 686-697. 

In other words, if an automated method can be considered equivalent in suitability in determining compliance, and if a compendial method does not require validation, then does it follow that an automated method using the same basic chemistry does not require validation of the original chemistry This puts automation closer to the same category... 

Tennant (T7) has also described an automated method using a Technicon continuous flow system and a short incubation time of 4 hours. Growth response of the organism to folate was estimated by measuring the rate of reduction of 2,3,5-triphenyl tetrazolium chloride. 

There are many dcliniiions of aulomalion. bui (he practical meaning is the performance of operations without human intervention. In the context of analytical chemistry, automation may involve operations like the preparation of samples, the measurement of responses, and the calculation of results. Tigure 3,1-1 illustrates the common steps in a typical chemical analysis and the automation methods used. In some cases, one or more of the steps shown on the left of the figure can be omitted. For example, if the sample is already a liquid, the dissolution step can he omitted. Likewise, if the method is highly selective, the separation step may be unnecessary. The steps listed in Figure 33-1 are sometimes called unit operations. 

In principal, synthesis route prediction can be done from scratch based on molecular calculations. However, this is a very difficult task since there are so many possible side reactions and no automated method for predicting all possible products for a given set of reactants. With a large amount of work by an experienced chemist, this can be done but the difficulty involved makes it seldom justified over more traditional noncomputational methods. Ideally, known reactions should be used before attempting to develop unknown reactions. Also, the ability to suggest reasonable protective groups will make the reaction scheme more feasible. 

Chemical kinetic methods of analysis continue to find use for the analysis of a variety of analytes, most notably in clinical laboratories, where automated methods aid in handling a large volume of samples. In this section several general quantitative applications are considered. 

Time, Cost, and Equipment Automated chemical kinetic methods of analysis provide a rapid means for analyzing samples, with throughputs ranging from several hundred to several thousand determinations per hour. The initial start-up costs, however, may be fairly high because an automated analysis requires a dedicated instrument designed to meet the specific needs of the analysis. When handled manually, chemical kinetic methods can be accomplished using equipment and instrumentation routinely available in most laboratories. Sample throughput, however, is much lower than with automated methods. 

The automated method differs from the ICSH method chiefly in that oxidation and ligation of heme iron occur after the hemes have been released from globin. Therefore, ferricyanide and cyanide need not diffuse into the hemoglobin and methemoglobin, respectively. Because diffusion is rate-limiting in this reaction sequence, the overall reaction time is reduced from approximately three minutes for the manual method to 3 —15 seconds for the automated method. Reaction sequences in the Coulter S + II and the Technicon H 1 and H 2 are similar. Moreover, similar reactions are used in the other Coulter systems and in the TOA and Unipath instmments. 

As computing capabiUty has improved, the need for automated methods of determining connectivity indexes, as well as group compositions and other stmctural parameters, for existing databases of chemical species has increased in importance. New naming techniques, such as SMILES, have been proposed which can be easily translated to these indexes and parameters by computer algorithms. Discussions of the more recent work in this area are available (281,282). SMILES has been used to input Contaminant stmctures into an expert system for aquatic toxicity prediction by generating LSER parameter values (243,258). 

In general, the advantages of using an automated method may be comparable to those of SA refinement in X-ray crystallography [68], where many of the operations necessary to refine a structure can be done automatically and the remaining manual interventions are easier because the SA refinement usually results in a more easily interpreted electron density map. Automated methods are usually used in combination with manual assignment. However, fully automated assignment of the NOEs is possible (see Eig. 7) [69]. 

Examples of strucmres for which automated assignment methods were used from the start are still rare [69,101]. However, automated methods are being used increasingly as a powerful tool in structure detennination in combination with manual assignment [102-105]. 

The continuous methods combine sample collection and the measurement technique in one automated process. The measurement methods used for continuous analyzers include conductometric, colorimetric, coulometric, and amperometric techniques for the determination of SO2 collected in a liquid medium (7). Other continuous methods utilize physicochemical techniques for detection of SO2 in a gas stream. These include flame photometric detection (described earlier) and fluorescence spectroscopy (8). Instruments based on all of these principles are available which meet standard performance specifications. 

The Micro-method uses an analytical instrument to measure Conradson carbon in a small automated set. The Micro-method (ASTM D4530) gives test results that are equivalent to the Conradson carbon residue test (D189). The purpose of this test is to provide some indication of relative coke forming tendency of such mat al. 

In two studies the cleansing and irritancy behavior of surfactants [106,107] were examined. An automated skin brushing method using a specific test soil and an epicutaneous irritation test on the dorsum of volunteers were applied. A sodium sulfosuccinate monoester based on a fatty alcohol ethoxylate gave very favorable results with respect to skin mildness although this concurred with low detergency. 

The soluble tryptic peptides of 130 mg a chain of Hb-St. Claude were separated on 0.9 x 60 cm columns of Chromobead resin type P (Technlcon Instruments, Dowex 50-X4) at 37°C using the procedure described earlier (16). The method uses a gradient of volatile pyrldlne-acetlc acid buffers of differing molarities and pH as follows first gradient, 666 ml 0.1 M, pH 3.1, and 333 ml 1.0 M, pH 5.0 and second gradient, 166 wl 1.0 M, pH 5.0, and 332 ml 2.0 M, pH 5.0. The amino acid composition of Isolated fragments was determined with a Splnco model 121 automated amino acid analyzer (Beckman Instruments)... 

New manual and automated method for determining activity of creatine kinase isoenzyme MB by use of dithiothreitol Clinical applications. Clin. Chem. (1975), 1612-1618. 

ChSS was fractionated on a column (550 x 15 mm) of DEAE Sepharo e Fast Flow using a Hiload System (Pharmacia), which was initially equilibrated in 0.005 M NaAc-bufFer pH 5.0. The sample was dissolved in water, the insoluble residue was removed by centrifugation and the supernatant was applied onto the column. After applying the gradient shown in Figure 1, the residual polysaccharides were washed from the column using 0.5 M NaOH. Fractions (23 ml) were collected and assayed by automated methods [2,3] for total neutral sugars and uronic acids. 

The SPARC (Sparc Performs Automated Reasoning in Chemistry) approach was introduced in the 1990s by Karickhoff, Carreira, Hilal and their colleagues [16-18]. This method uses LSER [19] to estimate perturbed molecular orbitals [20] to describe quantum effects such as charge distribuhon and delocalizahon, and polarizability of molecules followed by quanhtative structure-activity relationship (QSAR) studies to correlate structure with molecular properties. SPARC describes Gibbs energy of a given process (e.g. solvation in water) as a sum of ... 

A fully automated instrumental procedure has been developed for analyzing residual corrosion inhibitors in production waters in the field. The method uses ultraviolet (UV) and fluorescence spectrophotometric techniques to characterize different types of corrosion inhibitors. Laboratory evaluations showed that fluorescence is more suitable for field application because errors from high salinity, contamination, and matrix effect are minimized in fluorescence analysis. Comparison of the automated fluorescence technique with the classic extraction-dye transfer technique showed definite advantages of the former with respect to ease, speed, accuracy, and precision [1658],... 

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