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Is your T-shirt toxic? Some azo dyes can release carcinogenic amines after reductive cleavage of the azo bond. An example is acid red 114, which, following reduction, breaks down to o-tolidine (3,3-dimethylbenzidine). In Germany, these type of azo dyes are banned, and the toxic amines from the degradation products must not exceed 30 mg/kg of textile. Pakawadee Sutthivaiyakit of the Kasetsart University (Thailand) described an LC/MS/MS method with atmospheric pressure chemical ionization for the quantitative analysis of 20 of these unwanted amines. The research was done at the GSF National Research Center for Environment and Health (Germany) with Stefan Achatz and Antonius Kettrup. Textile sample extracts were reduced with sodium dithionite and cleaned using solid-phase extraction (following an official procedure) or with liquid–liquid extraction, which is a simpler process. One of the goals of method development was to obtain short total analysis times, and, therefore, the LC separation was performed on short columns in an isocratic mode. Peaks do overlap, says Sutthivaiyakit, but multireaction monitoring MS/MS allows selective detection of the compounds. In quadrupole mass spectrometer 1, a characteristic precursor is selected, then fragmented in quadrupole 2 by collision, and finally, the most abundant fragment is selected by quadrupole 3. This MS approach is limited to eight compounds at a time. Therefore, each sample extract undergoes three consecutive chromatographic runs with different MS conditions. Nevertheless, the total LC/MS/MS analysis time for all three runs is less than 15 min. For example, o-tolidine is identified by its retention time of about 4.5 min and characteristic ions at m/z 213, which is the precursor [M+H]+ ion, and m/z 196, which is the product ion after loss of NH3. Other toxic amines identified in this manner include benzidine, 2,4-diaminotoluene, 4,49-thiodianiline or 4-chloro-2methylaniline. Sutthivaiyakit plans now to establish the procedure at her university. Thailand has a big textile industry, and an efficient control of goods produced for export is of utmost importance.
Academic quality management Quality managers at a research center or in a university have a harder time than their colleagues in industry. In industry, there are clear guidelines or even government regulations on the analyses of commercial products. But what about analyses that are performed for internal clients or for a research project? Markus Krapp of the GKSS Research Centre (Germany) has found a way to establish a quality regimen at his institution. Some, but not all, laboratories and several individual procedures of the Centre are accreditated and, thus, monitored by external audits. Others follow Eurachem/Citac guidelines (e.g., “Quality Assurance for Research and Development and Non-Routine Analysis”). These documents are available on an internal, server-based quality information system, which includes listings of relevant Web sites, says Krapp. In addition, staff participate in various training programs, including a special course on quality assurance. The efforts are monitored by interlaboratory tests, internal audits, and quality management reviews. Documentation follows the Eurachem/Citac guidelines, which provides traceability and trackability. Krapp has introduced other quality management methods at the institution, including blank studies, control charts, intermethod comparisons, and determinations of measurement uncertainties. These types of quality assurance tools are typically unknown in research groups and especially in academia, he says. The effort could spread. Bernd Neidhart, also of GKSS, wants to establish such techniques widely in universities. Neidhart now chairs the Eurachem Working Group MAFIA, which translates to managing analytics for implementation in academia.
GOVERNMENT AND SOCIETY NACLA gains momentum The National Cooperation for Laboratory Accreditation (NACLA) announced at its second annual general meeting in April that efforts to reduce the number of accreditations for U.S. testing and calibration laboratories are well underway. Although participation is still lower than organizers had originally hoped, membership in NACLA reached 100 in January. Any organization that has an interest in laboratory accreditation in North America can apply for membership in NACLA in one of the following capacities—accreditor, government, laboratory, user of accreditation or laboratory services, or general interest. Membership in NACLA, however, does not guarantee recognition as a NACLA accrediting body. All accreditors will be evaluated according to NACLA recognition procedures. Thus far, four applications have been received from accrediting bodies, two of which had already undergone evaluations at the time of the meeting, and four more accrediting bodies are working to complete their applications. Recognition of the first group of accrediting bodies is expected this month. NACLA is a public–private partnership aimed at providing single
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accreditation with worldwide recognition for testing and calibration laboratories (Anal. Chem. 1997, 69, 161 A; 1999, 71, 314 A). NACLA is not intended to be another accrediting body, but rather a coordinator of accrediting bodies. Eventually, the organization hopes to expand to include accrediting bodies from Mexico and Canada, as well as the United States (NA would stand for North America instead of National). The goal is to establish procedures and criteria for laboratory accreditation and rules for reciprocal recognition. Ideally, the system would be accepted by all U.S. foreign trading partners. Although NACLA appears to be gaining momentum, several issues need to be hammered out before implementation can become a reality. High on the list is for Canada and Mexico to accept the NACLA procedures. Representatives from the Standards Council of Canada, the Canadian Standards Association, and EMA (an organization that integrates all laboratory accreditation in Mexico) have been observing NACLA’s progress from the sidelines but have not officially joined. Differences between NACLA’s guidelines and bylaws and those of the other organizations need to be reconciled before a merge can take place. As NACLA moves forward, it could also be merged with other organizations that have similar goals, such as the North American Calibration Cooperation (NACC) and the InterAmerican Accreditation Cooperation (IAAC), to form a North American contingent of the International Laboratory Accreditation Cooperation (ILAC). Whereas NACLA is focused on North America, ILAC is an international forum dedicated to the development of accreditation practices and procedures around the globe. Having a North American voice in ILAC and the world laboratory accreditation community would facilitate trade between Mexico, Canada, and the United States and provide North American laboratories with an opportunity to reduce the number of accredita-
tions, says Don Wilson of the Standards Council of Canada. On the down side, he says, there are several accreditation bodies already committed to and recognized by the Asia Pacific Laboratory Accreditation Cooperation (APLAC). Because of limited resources, accrediting bodies might not be able to join all regions. NACLA’s International Affairs Committee, chaired by Wilson, is working on a draft document, which would allow Canadian, Mexican, and U.S. programs under NACC to merge into the North American region of ILAC. IAAC may also be part of the arrangement. Another issue affecting many accreditation programs worldwide is incorporation of the new international standard, ISO/IEC 17025, which replaced Guide 25 in December 1999. A workshop was held in April after the annual meeting to bring NACLA participants up to speed on the changes involved. According to John Donaldson, vice president of the American National Standards Institute, ILAC is recommending a two-year transition period for laboratories to comply with the new 17025 requirements. Proficiency testing (PT) is one area that is not as clearly spelled out in 17025 as it is in Guide 25, says Martin Harper of the University of Alabama–Birmingham. NACLA organizers are currently working to develop an effective PT program, and they may now even have a bit more flexibility because of the new guidelines. Assessor training is also high on NACLA’s priority list. A training course for evaluators was held in March 1999, and another is planned for early 2001. NACLA is trying to expand the pool of available evaluators; currently there are only 14. NACLA is still soliciting members and volunteers to serve on committees. More information about the organization can be found on its Web site (http://ts.nist.gov/nacla). Britt Erickson
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of the Environment (DOE).
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