RESEARCH – DEVELOPMENT REPORT Project title: Improvment of methods and techniques for identification and determination at nanoscale of steroid structures contaminats in food Stage duration: December 2008 – November 2009 The objectives of the stage:
• Qualitative determination, based on retention times, the data of NIST libraries
of compounds or ionic fragments of contaminants with steroid structure
(estrone, beta-estradiol, cholesterol) in SIM or TIC mode;
• Application of derivatization in two stages (oximation and silylation) for
separation with significant resolution of contaminants hormone;
• The quantitative determination based on calibration curves with wide dynamic
range using a multicomponent stock solution of contaminant compounds with
steroid structure, organocloride pesticides and polychlorinated biphenyls in
• Application of SPE-GC-MS/MS experimental methodology, and SPE-GC-MS
for the extraction, concentration, separation, identification, quantification of
contaminants with steroid structure in real samples with different matrices;
• Application of special methods of extraction, purification and concentration on
polymer fiber (SPME) of steroids compounds in liquid samples (wastewater,
• Identification and determination by multirezidual analysis using liquid-liquid
extraction methods, of organocloride pesticides and polychlorinated biphenyls
in various food products (milk, grapes) by gas chromatographic techniques
coupled with electron capture detection (GC-ECD);
• Detection and quantification by mass spectrometry coupled with advanced
analytical techniques (gas chromatography, high performance liquid
chromatography): GC-MS, GC-MS/MS (with ion trap), LC-MS/MS, of
different steroids at the nanoscale level, in order to determination of
contaminants in complex matrices structures
Activities involved: A.2.1 Official trip to Eötvös Loránd University, Budapest
During 29.08-05.09.2009 Romanian team, consisting of chem. Lacrimioara
Senila, chem. Mirela Miclean and chem. Marin Senila, visited the Institute of Chemistry
of Eötvös Loránd University, Budapest. On this occasion, together with partner team
members (Professor Gyula Záray, Dr. Viktor Gábor Mihucz, Dr. Anikó Vasanits-Zsigrai,
Dr. András Helenkár) conducted a qualitative determination of:
o chemical compounds with steroid structure: ► estrone, ► β-estradiol, ►
cholesterol in samples with aqueous matrix, by the presentation of
fragmentation modes of complete derivatizated species of steroid
compounds and their derivatives trimethylsilyl ether / ester (oxime);
o qualitative determination of compounds with steroid structures: cholic
acids (cholic acid, acid litocholic, chenodeoxicholic acid, ursodeoxicholic
acid, 3-hydroxy 7-ketocolanic acid, dehidrocholic acid), from aqueous
samples by derivatized in two stages, then detection by gas
chromatography coupled with ion trap mass spectrometry (GC-MS/MS);
o qualitative determination of organochlorined pesticides (POC) and
polychlorinated biphenyls (PCBs) in food samples (milk and grape);
The investigation methods are: solid phase extraction (SPE) and liquid-liquid
extraction (LLE). SPE method is a very recent method involving derivatization in two
stages: oximation and silylation, gas chromatography coupled with detection by mass
spectromety with ion trap (GS/MS/MS), allowing residual multicomponent analysis by a
Qualitative determination of organochlorined pesticides (POC) and
polychlorinated biphenyls (PCBs) by injecting pure standards and real samples under the
same chromatographic conditions and comparing the retention times of analytes from the
pure standards with those from sample separated by chromatography column.
A.2.2 Receiving visit from the Eötvös Loránd University, Budapest
In 2009, ICIA Cluj-Napoca received visits of the Hungarian partner team, from
Eötvös Loránd University - Budapest. On these occasions a quantitative determination of:
organochlorined pesticides (OCPs) and polychlorinated biphenyls (PCBs) in food
samples (milk and grape) was conducted. Members of the two partner teams have visited
Lech Lacto SRL, in Lechinta, Bistriţa-Năsăud County, where they studied the processing
of milk and milk derivatives, and collected milk (raw and pasteurized) samples for OCPs
A.2.3 Activities foreseen in the research program of the young researcher
In the research program of the young researcher chem. Lacrimioara Senila the
methodologies for sample preparation prior to chromatographic determination were
developed, by performing the purification and concentration using:
and their application in different analysis for determination of the structure of compounds
contaminated with steroid (estrone, estradiol) and organoclorurate pesticides and
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Iliotibial band friction syndrome—A systematic reviewHealth Rehabilitation Research Centre, Division of Rehabilitation and Occupation Studies, Faculty of Health & Environmental Sciences, AUTUniversity, Private Bag 92006, Auckland, New ZealandReceived 19 October 2004; received in revised form 19 July 2006; accepted 30 August 2006Iliotibial band friction syndrome (ITBFS) is a common