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Limiting Dilution Assays for the Separation, Characterization, and Quantitation of Biologically Active Particles and Their Clonal Progeny

Authored by Carl Taswell, published in Cell Separation: Methods and Selected Applications, volume 4, chapter 6, pages 109-145, edited by Pretlow and Pretlow, 1987, Academic Press.

Following quote excerpted from the introduction of the review chapter:

I. INTRODUCTION

Since the beginning of this century, limiting dilution assays (LDAs) have been used to quantitate a wide variety of biologically active particles (BAPs) including bacteria (Phelps, 1908), protozoa (Cunningham, 1915), viruses (Clark, 1927), tumor cells (Hewitt, 1958), immunocompetent cells (Makinodan and Albright, 1962), and neurocompetent cells (Barbarese et al., 1983). LDAs can also be used to quantify the effectiveness of purification and depletion procedures (Taswell et al., 1979) and to separate and characterize BAPs and their clonal progeny (Taswell et al., 1980). Recent articles by Taswell (1981, 1984a,b) presented basic principles of LDAs, reviewed existing methods, and introduced new methods for the problems of model discrimination, parameter estimation, and design optimization. This article attempts to collect in one publication all methods of statistical analysis relevant to LDAs and to present them in a unified manner with a common terminology and notation.

Throughout most of their history, LDAs have been known as dilution assays, serial dilution assays, dilution series, dilution tests, fermentation tube tests, coliform density tests, etc., and limiting dilution analysis as the dilution method, dilution series method, fermentation tube technique, multiple tube method, multitube fermentation method, etc. It was only relatively recently that immunologists began using the newer terms "limiting dilution assays" (Kennedy et al., 1966) and "limiting dilution analysis" (Groves et al., 1970). Most bacteriologists, virologists, public health officials, and sanitary engineers still use the older terms (Wilson, 1983; Greenberg et al., 1985). Of all the different names for these bioassays, the term "limiting dilution assay (LDA)" is the most descriptive, the most general, and therefore the most appropriate for the collection of assays as a class. The words "limiting dilution" emphasize two important and related aspects of this class: (1) the assays are based on a process of dilution of the dose to extinction of the response, and (2) this process requires that only the BAP to be quantitated is diluted to these limiting doses while all other culture system constituents are provided at saturating (nonlimiting) doses.

Assuming that certain fundamental hypotheses (Section I,B) are validated for each case, the same methods of statistical analysis apply to all LDAs regardless of the kind of BAP diluted in liquid suspension. Indeed, these methods also apply to procedures used to quantitate BAPs that are not suspended in liquid. Botanists, ecologists, and foresters quantitate plants on tracts of land; their observational studies analogous to LDAs are called stocked-quadrat surveys (Blackman, 1935; Swindel, 1983). Agricultural and veterinary scientists quantitate viruliferous insects in a vector population capable of transmitting viral, bacterial, fungal, or parasitic diseases to plant and animal hosts; their experimental procedures analogous to LDAs are apparently not known by any particular name (Thompson, 1962; Kerr, 1971). All of these LDAs and analogous procedures are dose–response assays that detect quantal responses and require dilution of the dose to extinction of the response. They must be distinguished from a related class of assays (such as plate, colony, plaque, and pock count assays) that detect quantitative responses and do not require dilution to extinction. Different methods of statistical analysis apply to this related but distinct class of assays (Fisher et al., 1922; Roberts and Coote, 1965). These methods cannot be used for LDAs.

A. Limiting Dilution Assays (LDAs)

LDAs detect binary (positive or negative) responses generated by BAPs in individual in vivo or in vitro cultures within groups of replicate cultures that vary in the dose of the test preparation from which the BAPs are sampled. LDAs can be used to estimate the absolute number of BAPs [called the most probable number, MPN, or density of coliform organisms by bacteriologists (Phelps, 1908; Wilson, 1983)], the 50% endpoint on the dilution scale of the BAP test preparation [the dilution level at which the group of replicates is 50% positive and 50% negative (Reed and Muench, 1938; Worcester, 1954)], and the relative frequency of BAPs [called the immunocompetent cell frequency by immunologists (Taswell, 1981)]. These three parameter estimates are obtained from two subclasses of LDAs: subclass I consists of all LDAs that can be used to calculate absolute numbers and 50% endpoints but not relative frequencies, and subclass II consists of all LDAs that can be used to calculate all three parameter estimates. Absolute numbers are expressed as the number of BAPs per unit volume of test preparation, 50% endpoints as units on the dilution scale of the BAP test preparation, and relative frequencies as the proportion of BAPs within a mixture of biologically active and inactive particles (BAPs and BIPs), Dilution levels for 50% endpoints may be necessary for drug or antisera titration studies but not appropriate for any study where it is possible and meaningful to estimate the absolute number of BAPs (because a dilution level is clearly less informative than an absolute number). Therefore, they will not be considered further in this article.

The two subclasses can then be designated by their distinguishing parametric estimates as absolute number LDAs (subclass I) and relative frequency LDAs (subclass II). Both absolute number and relative frequency LDAs are biological assays for particles of a specific type defined by their functional activity and called biologically active or assayable particles (BAPs). Relative frequency LDAs, however, also incorporate an accompanying physicochemical assay for particles of a general type defined by their structural morphology or other physicochemical characteristics and called physicochemically observable particles (POPs). As an example, LDAs are used to measure the relative frequency of cytolytic T lymphocyte precursors (CTL-Ps) as the BAPs within a mixture of leukocytes as the POPs (Taswell et al., 1979). In this example, the functional activity of the BAPs is defined as cell differentiation and proliferation producing a clone of cells that can kill target cells (assayed indirectly by 51Cr release), while the structural morphology of the POPs is defined as standard leukocytic morphology (observed directly by light microscopy). In absolute number LDAs, the number of POPs (theoretically equal to the number of BAPs plus BIPs) is never known because any physicochemical assay that could conceivably be used to observe them is not performed due to impracticality or impossibility.

B. The Single-Hit Poisson Model (SHPM)

To analyze dose–response data from LDAs, it is necessary to validate a model incorporating two fundamental hypotheses: one for the provision of the dose and the other for the generation of the response. For the sampling of BAPs aliquoted to replicate cultures, first McCrady (1915) assumed a binomial distribution hypothesis and then Greenwood and Yule (1917) a Poisson distribution hypothesis. For the generation of a ...

Following quote excerpted from the conclusion of the review chapter:

IX. CONCLUSION

LDAs were originally developed and have been most extensively used by public health officials and sanitary engineers for the examination of water supplies, sewage and waste water, and dairy products (Phelps, 1908; McCrady, 1915; Greenwood and Yule, 1917; Greenberg et al., 1985; Richardson, 1985). As discussed in Section I, LDAs have also been used by investigators from many other biological and medical sciences. It is the immunologists, however, who have been responsible for renewing interest over the past decade in the continuing development of methods for the statistical analysis of LDA data. This renewed interest derives from the increased size of assays and complexity of applications in immunology. Sanitary engineers typically use 1, 5, or 10 replicates for each of from 1 to 3 dose groups to determine, for example, whether the concentration of bacteria in drinking water does not exceed the maximum safe level. Immunologists, however, typically use, say, 24, 60, 192, or more replicates for each of from 3 to 6 or more dose groups to perform experimental comparisons, clonal analyses, and partition analyses (Sections VI, VII, and VIII, respectively) that are relatively much more complicated. Renewed interest in statistical research for LDAs also derives from advances in computers and statistics. Efficient statistical analysis of data from larger, more complicated assays would never have been practically feasible without the assistance of the powerful yet economical personal computers that have become available just within the past decade. Many new theories and methods have been developed in statistics over the past several decades, some that have been and some that have not yet been applied to LDAs, as discussed throughout this article. Certainly, much work remains to be done.

This article attempts to provide an outline of all statistical methods relevant to LDAs, reviewing past origins and recommending future directions. Apparently, it is the first such attempt to collect statistical work on LDAs from many diverse fields and to unify it with a common terminology and notation within a systematic treatment of validity tests, parameter estimators, and assay design for both sample and population LDAs. Hopefully, it will not be the last such attempt. The distinction between sample and population LDAs (Section I,C) and the boundary between the concepts of using sample LDAs to estimate sample parameters (Section III) and population LDAs to estimate both sample and population parameters (Section IV,B) should be explored further. These issues of parameter estimation should be investigated within a conceptual framework that fully integrates model discrimination and selection (Sections II and IV,A) and design optimization (Section V). The goal of this approach should be to extract maximum information from past assays in a sequence in order to obtain maximum information from future assays in the sequence. Furthermore, it should also be to estimate the biological variance ... of the samples ... within the population in addition to the usual statistical variance ... of the sample estimator ... given the sample ... A method for estimating ... [the biological variance of the samples] ... is introduced for the first time in this article (Section IV,B), and examples are provided with estimates of the biological variance between samples within the same population for several different populations (Section VI). Estimation of ... [the variance between samples]... will enable investigators to better characterize their study populations by quantitating the biological variation between the BAP frequencies of test preparations from individual mice, patients, or other sources. LDAs have been used for almost a century now. They have proved to be valuable tools in the hands of biological and medical scientists for the separation, characterization, and quantitation of BAPs and their clonal progeny. Continuing development and proper use of new methods of statistical analysis for LDAs can only serve to enhance the power of these tools.


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