Compliance analytical

This chapter highlights the important aspects of the analytical transfer process as they relate to compliance, analytical data, and documentation. Other chapters in this text should be consulted for elaboration on the various important facets of technical transfer, including method development, method validation, documentation, and stability. 

Another application for which biosensors may prove useful is in the post-closure groundwater monitoring. After wells have been established, monitoring must continue (in some cases mandated by law) even though the contamination has been contained, and samples are consistently returned from laboratory analysis as non-detects. In these cases, a sentinel capability which could continuously monitor for non-compliance analyte concentrations would be highly cost-effective. 

This chapter highlights the important aspects of the analytical transfer processes as they relate to process, compliance, analytical data, and documentation. Types of method transfers and the timeline of transfer activities are discussed. The risk assessment prior to initiation of transfer activities is also described. The chapter describes content and utility of the transfer protocol and final report, as well as documents that govern analytical method transfers (i.e., SOPs and master plan). The importance of selecting appropriate method transfer acceptance criteria and use of statistical methods to evaluate results are described. The significance of the inclusion of an adequate level of detail in the methods, protocol(s), and other documents cannot be overly stressed. Last of all, the process for transfer of technical ownership of the analytical methods is discussed. Other chapters in this text should be consulted for elaboration on the various important facets of technical transfer, including method development, method validation, documentation, and stability. 

The objective of the FCC is to define food-grade chemicals in terms of the characteristics that estabUsh identity, strength, and quahty. It provides specifications in monograph form for some 900 food additives, together with analytical test procedures by which compliance with the specifications can be determined. The third edition was pubUshed in 1981 supplements followed in 1983, 1986, 1991, and 1993. The fourth edition is in preparation as of this writing and is to include monographs for almost 1000 food chemicals, including flavors. 

Operations capable of generating airborne beryUium particulate, such as melting, machining, welding, grinding, etc, are effectively controUed by local exhaust ventilation or other control measures. To assure a safe environment and measure compliance with the OSHA standards, employee exposures should be periodicaUy measured by prescribed air sampling and analytical methods. 

The effect of such well-intentioned regulations might be counterproductive Industry could either be forced to withdraw products from the market despite their scientific merits because compliance is impossible, or they might dishonestly propose analytical methods that sweep all but a scapegoat impurity below the carpet. 

Data concerning use patterns of food additives and color additives are difficult to obtain. Although additives must be included on product labels in descending order of inclusion, major effort is required to evaluate even a simple presence on this basis, which would provide at best only limited information on the amounts used. In most cases, quantitative analytical controls are limited to efforts by control authorities to determine compliance with legal limits. Levels below these limits are of limited interest and are usually not published. ... 

As with urine, saliva (spumm) is easy to collect. The levels of protein and lipids in saliva or spumm are low (compared to blood samples). These matrices are viscous, which is why extraction efficiency of xenobioties amoimts to only 5 to 9%. By acidifying the samples, extraction efficiencies are improved as the samples are clarified, and proteinaceous material and cellular debris are precipitated and removed. Some xenobioties and their metabohtes are expressed in hair. Hair is an ideal matrix for extraction of analytes to nonpolar phases, especially when the parent xenobioties are extensively metabolized and often nondetectable in other tissues (parent molecules of xenobioties are usually less polar than metabolites). Hair is a popular target for forensic purposes and to monitor drug compliance and abuse. Human milk may be an indicator of exposure of a newborn to compounds to which the mother has been previously exposed. The main components of human milk are water (88%), proteins (3%), lipids (3%), and carbohydrates in the form of lactose (6%). At present, increasing attention is devoted to the determination of xenobioties in breath. This matrix, however, contains only volatile substances, whose analysis is not related to PLC applications. 

Wilder, D. R., New directions in industrial environmental analytical chemistry beyond compliance testing, Crit. Rev. Anal. Chem., 25, 77, 1989. 

It should be mentioned that the Food Additives Analytical Manual (FAAM) [75] provides analysts with FDA evaluated methodology (partly subjected to collaborative study) needed to determine compliance with food additive regulations, including procedures for indirect food additives, such as butylated hydroxy-anisole (BHA), butylated hydroxytoluene (BHT), t-butylhydroxyquinone (TBHQ), dilaurylthiopropionate (DLTDP), fatty acid methyl esters (FAME), sodium benzoate, sorbitol, and others. 

Analytical methods for 12 chlorinated phenolics and adsorbable organic halides (AOXs). Samples of air emissions and water discharges from each mill must be tested using the laboratory methods included in the rule. The new methods will enable more timely and accurate measurements of releases of these pollutants to the environment and will be used to ensure compliance with air emission and water discharge permit limits... 

In general, the question you should always ask is, What will the results of the analysis be used for . If you are sampling for compliance with a contractual requirement, i.e. the sample must contain a minimum/maximum amount of the analyte, then it is important to know how this is interpreted. At the time of writing, the Codex Alimentarius Commission recommended the following limits for food-grade salt [12] ... 

ISO has two important functions in analytical chemistry. The first is to publish descriptions of accepted methods. These are effectively industry standard methods for particular protocols. The second is in laboratory accreditation. For a laboratory to be ISO accredited, compliance with international QA standards must be confirmed by an initial assessment and subsequently from repeated audits by an independent assessor. Since ISO has no legal or regulatory powers, the standards are voluntary. It is unlikely, however, that a forensic analysis which did not conform to an ISO standard would be upheld in court, for example. Most commercial laboratories need to be accredited to remain competitive and to deal with regulatory authorities. Most university labs are not accredited, mainly due to the time and costs involved, and also to the nonroutine nature of much university research. However, university accreditation may become a requirement in the near future, especially for publicly funded research in the UK. The details of laboratory accreditation are discussed by Christie et al. (1999) and Dobb (2004). 

By using the combination of specific method accreditation and generic accreditation it will be possible for laboratories to be accredited for all the analyses of which they are capable and competent to undertake. Method performance validation data demonstrating that the method was fit-for-purpose shall be demonstrated before the test result is released and method performance shall be monitored by on-going quality-control techniques where applicable. It will be necessary for laboratories to be able to demonstrate quality-control procedures to ensure compliance with the EN 45001 Standard,3 an example of which would be compliance with the ISO/AOAC/IUPAC Guidelines on Internal Quality Control in Analytical Chemistry Laboratories.12... 

ISO, IUPAC and AOAC INTERNATIONAL have co-operated to produce agreed protocols on the Design, Conduct and Interpretation of Collaborative Studies 14 and on the Proficiency Testing of [Chemical] Analytical Laboratories .11 The Working Group that produced these protocols has prepared a further protocol on the internal quality control of data produced in analytical laboratories. The document was finalised in 1994 and published in 1995 as the Harmonised Guidelines For Internal Quality Control In Analytical Chemistry Laboratories .12 The use of the procedures outlined in the Protocol should aid compliance with the accreditation requirements specified above. 

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