news from analytica 2000: is your t-shirt toxic?

1
JUNE 1, 2000 / ANALYTICAL CHEMISTRY 393 A n ews 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 bod- ies, two of which had already undergone evaluations at the time of the meeting, and four more accrediting bodies are working to com- plete their applications. Recognition of the first group of accrediting bodies is expected this month. NACLA is a public–private partnership aimed at providing single Is yourT-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-toli- dine (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 ex- traction (following an official procedure) or with liquid–liquid extraction, which is a sim- pler process. One of the goals of method development was to obtain short total analy- sis times, and, therefore, the LC separation was performed on short columns in an isocrat- ic 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 NH 3 . Other toxic amines identified in this manner include benzidine, 2,4-diamino- toluene, 4,49-thiodianiline or 4-chloro-2- methylaniline. 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 com- mercial 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 interlabo- ratory tests, internal audits, and quality management reviews. Docu- mentation 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 com- parisons, 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 manag- ing analytics for implementation in academia. GOVERNMENT AND SOCIETY

Upload: veronika

Post on 22-Feb-2017

213 views

Category:

Documents


0 download

TRANSCRIPT

Page 1: News from Analytica 2000: Is your T-shirt toxic?

J U N E 1 , 2 0 0 0 / A N A LY T I C A L C H E M I S T R Y 3 9 3 A

n ews

NACLA gains momentum

The National Cooperation for Laboratory Accreditation (NACLA)announced at its second annual general meeting in April that efforts toreduce the number of accreditations for U.S. testing and calibrationlaboratories are well underway. Although participation is still lowerthan organizers had originally hoped, membership in NACLA reached100 in January.Any organization that has an interest in laboratory accreditation in

North America can apply for membership in NACLA in one of thefollowing capacities—accreditor, government, laboratory, user ofaccreditation or laboratory services, or general interest. Membershipin NACLA, however, does not guarantee recognition as a NACLAaccrediting body. All accreditors will be evaluated according toNACLA recognition procedures.Thus far, four applications have been received from accrediting bod-

ies, two of which had already undergone evaluations at the time ofthe meeting, and four more accrediting bodies are working to com-plete their applications. Recognition of the first group of accreditingbodies is expected this month.NACLA is a public–private partnership aimed at providing single

Is yourT-shirt toxic?

Some azo dyes can release carcinogenicamines after reductive cleavage of the azobond. An example is acid red 114, which,following reduction, breaks down to o-toli-dine (3,3-dimethylbenzidine). In Germany,these type of azo dyes are banned, and thetoxic amines from the degradation productsmust not exceed 30 mg/kg of textile.Pakawadee Sutthivaiyakit of the Kasetsart

University (Thailand) described an LC/MS/MSmethod with atmospheric pressure chemicalionization for the quantitative analysis of 20of these unwanted amines. The research wasdone at the GSF National Research Centerfor Environment and Health (Germany) withStefan Achatz and Antonius Kettrup. Textilesample extracts were reduced with sodiumdithionite and cleaned using solid-phase ex-traction (following an official procedure) orwith liquid–liquid extraction, which is a sim-pler process. One of the goals of methoddevelopment was to obtain short total analy-sis times, and, therefore, the LC separationwas performed on short columns in an isocrat-ic mode. Peaks do overlap, says Sutthivaiyakit,but multireaction monitoring MS/MS allowsselective detection of the compounds.In quadrupole mass spectrometer 1, a

characteristic precursor is selected, thenfragmented in quadrupole 2 by collision,and finally, the most abundant fragment isselected by quadrupole 3. This MS approachis limited to eight compounds at a time.Therefore, each sample extract undergoesthree consecutive chromatographic runswith different MS conditions. Nevertheless,the total LC/MS/MS analysis time for allthree runs is less than 15 min. For example,o-tolidine is identified by its retention timeof about 4.5 min and characteristic ions atm/z 213, which is the precursor [M+H]+ ion,and m/z 196, which is the product ion afterloss of NH3. Other toxic amines identified inthis manner include benzidine, 2,4-diamino-toluene, 4,49-thiodianiline or 4-chloro-2-methylaniline.Sutthivaiyakit plans now to establish the

procedure at her university. Thailand has abig textile industry, and an efficient controlof goods produced for export is of utmostimportance.

Academic quality management

Quality managers at a research center or in a university have a hardertime than their colleagues in industry. In industry, there are clearguidelines or even government regulations on the analyses of com-mercial products. But what about analyses that are performed forinternal 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 notall, laboratories and several individual procedures of the Centre areaccreditated and, thus, monitored by external audits. Others followEurachem/Citac guidelines (e.g., “Quality Assurance for Researchand Development and Non-Routine Analysis”). These documentsare 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 specialcourse on quality assurance. The efforts are monitored by interlabo-ratory tests, internal audits, and quality management reviews. Docu-mentation follows the Eurachem/Citac guidelines, which providestraceability and trackability.Krapp has introduced other quality management methods at the

institution, including blank studies, control charts, intermethod com-parisons, and determinations of measurement uncertainties. Thesetypes of quality assurance tools are typically unknown in researchgroups 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 chairsthe Eurachem Working Group MAFIA, which translates to manag-ing analytics for implementation in academia.

GOVERNMENT AND SOCIETY