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Eterična ulja su smjese hlapljivih, lipofilnih tvari izoliranih iz cijelih biljaka ili njihovih dijelova. Lako su pokretljive tekućine koje lome svjetlo, bezbojne su ili svijetložute boje i najčešće su intenzivnog mirisa koji ovisi o kemijskom sastavu ulja. Koriste se zbog antibakterijskog, antivirusnog, antimikotičkog, antiparazitskog, spazmolitičkog, protuupalnog i antikancerogenog djelovanja, pogotovo u farmaceutskoj, kozmetičkoj, poljoprivrednoj i prehrambenoj industriji. Hidrolati su vodene otopine zasićene sastavnicama eteričnog ulja koje mogu nastati kao nusprodukt destilacije hlapljivih ulja ili destilacije biljnog materijala koji ne sadrži hlapljiva ulja. Blagi su, neiritativni i neškodljivi u usporedbi s eteričnim uljima. Upotrebljavaju se u kozmetici kao tonici za kožu te vodene faze krema i maski, a u terapiji u obliku obloga, kapi za nos, za oralnu upotrebu i primjenu na sluznice te u nekim zemljama kao pića, arome ili u fitomedicini. Određena količina sakupljenog suhog biljnog materijala se koristila za vodenu destilaciju uz pomoć aparature po Clevengeru da bi se izolirala eterična ulja i hidrolati. Zatim je odrađena GC-MS i GC-FID analiza da bi se dobio točan sastav eteričnih ulja i hidrolata. Iz tih rezultata se može vidjeti da su eterična ulja izrazito nepolarna i lipofilna, za razliku od hidrolata koji su polarniji, tako da se i njihov međusobni sastav razlikovao, iako smo našli zajedničke spojeve u visokim udjelima (heksadekanska kiselina, heksahidrofarnezil aceton, fitol i heptakosan)., Essential oils are mixtures of volatile, lipophilic substances isolated from whole plants or their parts. They are easily moving liquids that refract light, are colorless or light yellow in color and are most often of intense odor, which depends on the chemical composition of the oil. They have been used for antibacterial, antiviral, antimycotic, antiparasitic, antispasmodic, anti-inflammatory and anticancer activities, especially in the pharmaceutical, cosmetic, agricultural and food industries. Hydrosols are aqueous solutions saturated with constituents of essential oil that can be produced as a by-product of the distillation of volatile oils or the distillation of a plant material that does not contain volatile oils. They are mild, non-irritating and harmless compared to the essential oils. They are used in cosmetics as skin tonics and the aqueous phases of creams and masks, and in therapy in the form of dressings, nasal drops, oral and mucosal applications, and in some countries as beverages, flavors or in phytomedicine. A certain amount of dried plant material was used for aqueous distillation using a Clevenger apparatus to isolate essential oils and hydrosols. Then, GC-MS and GC-FID analysis were performed to obtain the correct composition of essential oils and hydrosols. From these results it can be seen that the essential oils are highly non-polar and lipophilic, unlike the more hydrosols, which are more polar, so that their mutual composition differed, although we found common compounds in high proportions (hexadecanoic acid, hexahydrofarnasyl acetone, phytol and heptacosane).

Ciljevi ispitivanja: Cilj ovog eksperimentalnog rada je bio je pmomoću GC-MS metode kvantitativno odrediti koncentracije nikotina i kotinina i trans-3- hdroksikotinina u biološkim uzorcima urina dobrovoljnih ispitanika prije i poslje odlaksa u noćni klub u kojem je dozvoljeno pušenje. Materijal i metode: U straživanju je sudjelovalo 22 ispitanika, od toga 7 muškaraca i 15 žena. Biološki uzorci urina nepoznath koncentracija nikotina i metabolita pripremljen za analizu ekstrakcijskom metodom tekuće-tekuće (LLE).Za analizu koristili smo GC-MS. Rezultati: Svi uzorci bili su pozitivni na nikotin i metabolite. Srednja vrjednost nikotina, kotinina i 3-OHK prije izloženosti u noćnom klubu kod nepušača iznosila je 8,197 ng/mL, 28,372 ng/mL, 12,303 ng/mL kod žena i 11,235 ng/mL, 25,763 ng/mL, 3,673 ng/mL kod muškaraca. Srednja vrijednost nakon izloženosti iznosila je: 123,373 ng/mL, 56,544 ng/mL, 41,501 ng/mL kod žena i 21,366 ng/mL, 65,234 ng/mL, 14,941 ng/mL kod muškaraca. Zaključci: Koncentracije nikotina i metabolita kod nepušača prije izloženosti bile su značajn manje neko nakon izloženosti. Razine nikotina i metabolita kod pušača značajn su veće nego li kod nepušaća. S obzirom a dužinu izloženost porast koncentracija kod konobara, nepušača za nikotin, kotinin i 3-OHK veći je neko kod muških ispitanika koji su boravili u klubu kao posjetitelji., Aims of the study: The purpose of this experimental work was to quantitatively determine the concentrations of nicotine and cotinine and trans-3-hydroxycotinine in biological urine samples from voluntary subjects before and after their visit to a nightclub in which smoking was allowed, by using the GC-MS method. Material and methods: Twenty-two subjects participated in the research, including 7 men and 15 women. Biological urine samples of unknown nicotine and metabolite concentrations were prepared for analysis by the liquid-liquid extraction (LLE) method. For analysis, we used the GC-MS method. Results: All samples were positive for nicotine metabolites. The mean value of nicotine, cotinine and 3-OHK before exposure at a nightclub in non-smokers was 8,197 ng / mL, 28,372 ng / mL, 12,303 ng / mL in women and 11,235 ng / mL, 25,763 ng / mL, 3,673 ng / mL in men. Mean post-exposure values were: 123,373 ng / mL, 56,544 ng / mL, 41,501 ng / mL in women and 21,366 ng / mL, 65,234 ng / mL, 14,941 ng / mL in men. Conclusions: Concentrations of nicotine and metabolites in non-smokers before exposure were significantly lower than after exposure. The levels of nicotine and metabolites in smokers are significantly higher than in non-smokers. Considering the length of exposure, the increase in concentrations of nicotine, cotinine, and 3-OHK in non-smoker waiters was higher than in male respondents who stayed in the club as visitors.

Ciljevi istraživanja: Razviti metodu za određivanje koncentracija nikotina i njegovih metabolita i biološkom uzorku urina pomoću izrade baždarnih krivulja otopina referentnih standarda poznatih koncentracija te pomoću njih izračunati nepoznate koncentracije u uzorcima urina u kojima su koncentracije nikotina i metabolita nepoznate. Odrediti validacijske parametre navedene metode. Ustroj istraživanja: Eksperimentalna studija Mjesto istraživanja: Kemijsko-toksikološki laboratorij Kliničkog odjela za sudsku medicinu Zavoda za patologiju, sudsku medicinu i citologiju, Kliničkog bolničkog centra u Splitu. Materijal i metode: Otopine za izradu baždarne krivulje dobivene su serijskim razrjeđivanjem referentnih standarda, prvo u metanolu te zatim u uzorku urina, nakon čega su uzeti jednaki volumeni istih koncentracija sve tri tvari te smo pokrili veće koncentracijsko područje. MIX otopine standarda su ekstrahirani metodom tekuće-tekuće (LLE), razrijeđeni kloroformom i analizirani plinskom kromatografijom s masenim spektrometrom snimanjem ukupne ionske struje (TIC). Nakon izrade baždarnih krivulja, slijedi njihova primjena u određivanju koncentracije nikotina i metabolita u realnim uzorcima urina. Rezultati: Umjerne krivulje za nikotin, kotinin i 3-hidroksikotinin uspješno su napravljene pomoću dobivenih signala ciljanim mjerenjem otopina standarda u urinu pri koncentracijama od 0,3-1000 ng/mL. Dokazana je linearnost metode sa koeficjentom korelacije R>0,99. Ponovljivost također zadovoljava kriterij prihvatljivosti (RSD, Objectives: The objective of this study was to develop a method for simultaneous concentration determination of nicotine and its metabolisms in biological urine sample by making calibration curves using reference standard solutions of known concentrations to calculate unknown concentrations in urine samples. Determine the validation parameters of the specified method. Design: Experimental study Settings: Laboratory of Toxicology, Department of pathology, forensic medicine and cytology, University Hospital of Split. Material and Methods: Calibration solutions were obtained by serial dilution of the reference standards, first in methanol and then in a urine sample, after which equal volumes of the same concentrations of all three substances were taken and a larger concentration area was covered. MIX solutions of the standards were extracted by liquid-liquid (LLE) method, diluted with chloroform and analyzed by total ion current (TIC) gas chromatography with mass spectrometer. After the preparation of the calibration curves, their application is followed in the determination of the concentration of nicotine and metabolites in real urine samples. Results: Calibration curves for nicotine, cotinine, and 3-OH-cotinine were successfully constructed using the obtained signals by the targeted measurement of standard solutions in urine at concentrations of 0.3-1000 ng/mL. The linearity of the method with a correlation coefficient R> 0.99 was proved. Repeatability also meets the eligibility criterion (RSD

Ciljevi istraživanja: Kvalitativna analiza dječjih krema, usporedba dobivenih rezultata s deklaracijom proizvoda te pronalazak poveznice između cijene proizvoda i prisusCiljevi istraživanja: Kvalitativnom analizom ispitati sastav dječjih šampona i kupki, usporediti navode deklaracije s dobivenim rezultatima, ispitati prisustvo štetnih sastojaka te prikazati korelaciju dobivenih rezultata s mjestom prodaje proizvoda. Materijali i metode: Ispitano je 10 uzoraka dječjih šampona i kupki. Za analitičku pripremu uzoraka korištene su staklene Petrijeve zdjelice na koje je nanesen uzorak mase 0,1 g. Uzorci su ekstrahirani smjesom organskih otapala: kloroforma, etil acetata i N-heksana u jednakom omjeru. Kvalitativna analiza je izvršena GC-MS metodom. Za usporedbu otapala uzorak 1 otopljen je i u čistom kloroformu. Rezultati: Kvalitativnom analizom u uzorcima je detektirano u rasponu 19-54 supstanci, dok ih je na pojedinačnim deklaracijama navedeno u rasponu 12-25. Posebno je ispitivano prisustvo štetnih sastojaka: parabena, dietilftalata, fenoksietanola te metilizotiazolinona. Metilizotiazolinon nije detektiran u nijednom uzorku, iako je deklariran u uzorku 6. Od ukupno 10 ispitivanih uzoraka, u 4 uzorka je dokazano prisustvo nepoželjnih sastojaka. U samo jednom uzorku detektiran je paraben. Prisutnost ftalata detektirana je u svim uzorcima, međutim jedino kod uzorka 9 smatra se da nije rezultat onečišćenja. Usporedbom kromatograma uzorka 1, dokazano je da smjesa organskih otapala daje jasnije signale u odnosu na sami kloroform. Zaključak: Ovim istraživanjem pokazano je odstupanje deklaracija u prosjeku od 12 supstanci. Podudarnost deklaracija s brojem detektiranih tvari pokazala se najlošijom kod proizvoda dostupnih isključivo u ljekarnama i specijaliziranim prodavaonicama, no upravo u navedenim proizvodima detektirano je najmanje štetnih sastojaka. Od 4 uzorka iz linije za poseban tip kože, za 3 je pokazano da odgovaraju svojoj namijeni., Objectives: Qualitative determination of ingredients in baby shampoos and baths, as well as the comparison of the results with declarations. Examine the presence of harmful ingredients and to find a correlation between the place of product sales and obtained results. Materials and methods: Ten samples of baby shampoos and baths were examined. Samples were extracted with a mixture of organic solvents, chloroform, ethyl acetate and N-hexane in equal proportions. Qualitative analysis was performed by a GC-MS method. For comparison of the results, sample 1 was dissolved in pure chloroform. Results: By qualitative analysis of the samples 19-54 substances were detected, while 12-25 substances were listed on each declarations. The presence of harmful substances such as parabens, diethyl phthalates, phenoxyethanol and methylisothiazolinone was investigated. Methylisothiazolinone was not detected in any of the samples, although it was declared in sample No. 6. Out of a total of 10 tested samples, 4 samples showed the presence of undesirable ingredients. Paraben was detected in only one sample. The presence of phthalate was detected in all samples, but only in sample 9 it is considered not to be the result of contamination. By comparing chromatograms of sample 1, it was shown that the mixture of organic solvents gave clearer signals relative to the chloroform itself. Conclusion: This study showed a deviation of the declaration on an average of 12 substances. The conformity of the declaration compared with the number of detected substances was the worst in products available only in pharmacies and specialized stores, but the least harmful ingredients were detected in these products. Of the 4 samples from the line for a special type of skin, for 3 is shown to suit their purpose.

Ciljevi istraživanja: Razviti metodu za simultano određivanje koncentracija pet sintetskih katinona (bufedrona, mefedrona, DMMC-a, pentilona i MDPV-a) u mokraći, koja podrazumijeva izradu umjernih krivulja te njihovu primjenu na uzorcima u kojima su koncentracije nepoznate. Materijal i metode: Otopine sintetskih katinona za izradu umjerne krivulje dobivene su serijskim razrjeđivanjem referentnih standarda u mokraći te su zajedno ekstrahirane i pripremljene za analizu. Koncentracije bufedrona, mefedrona, DMMC-a, pentilona i MDPV-a određivale su se u dvama uzorcima mokraće u koje su dodani različiti nepoznati volumeni pripravljenih standardnih otopina. Ekstrahirani su metodom tekuće-tekuće (LLE), razrijeđeni kloroformom i analizirani tehnikom GC-MS snimanjem ukupne ionske struje (TIC). Rezultati: Kvantitativnom analizom sintetskih katinona pri 4000 ng/mL dobiveni su podaci o njihovim karakterističnim retencijskim vremenima (RT) i spektrima masa. Umjerne krivulje za simultano dokazivanje spomenutih sintetskih katinona uspješno su konstruirane pomoću dobivenih signala ciljanim mjerenjem otopina standarda u mokraći pri koncentracijama 200-4000 ng/mL. U oba biološka uzorka detektirani su svi sintetski katinoni te su očitane njihove nepoznate koncentracije. Prisutnost bufedrona, mefedrona, DMMC-a, pentilona i MDPV-a u oba uzorka mokraće potvrđena je i nakon derivatizacije. Zaključci: Razvijena je i provjerena GC-MS metoda primjenjiva za simultanu kvalitativnu i kvantitativnu analizu bufedrona, mefedrona, DMMC-a, pentilona i MDPV-a u biološkim uzorcima mokraće. To ima veliku važnost jer se sintetski katinoni brzo šire na globalnom tržištu. Daljnja istraživanja trebala bi uključiti veći broj sintetskih katinona i više vrsta bioloških uzoraka za dokazivanje njihovog prisutstva., Objectives: The objective was to develop a method for simultaneous concentration determination of five synthetic cathinones in urine (buphedrone, mephedrone, DMMC, pentylone and MDPV), which implies plotting calibration curves and applying them to determine unknown concentrations in urine samples. Material and methods: In order to make the solutions of chosen synthetic cathinones used for creating calibration curves, serial dilution of reference standard solutions was made in a blank urine sample. Synthetic cathinones were extracted jointly and prepared for analysis. After adding different unknown volumes of standard solutions to two urine samples, unknown concentrations were determined. Liquid-liquid technique was used for the extraction of samples, followed by dilution in chloroform to prepare for a GC-MS analysis. The chosen working mode was total ion current (TIC). Results: Information about retention times (RT) and mass spectra of synthetic cathinones was obtained by qualitative analysis of concentration 4000 ng/mL. Calibration curves were successfully constructed using peak signals obtained by analysing concentrations 200-4000 ng/mL. In both urine samples all synthetic cathinones were detected and their unknown concentrations were determined. Their presence in both urine samples was additionally confirmed after derivatization. Conclusion: A GC-MS method applicable to simultaneous qualitative and quantitative analysis of buphedrone, mephedrone, DMMC, pentylone and MDPV in urine samples has been developed and tested. Such method development is valuable because synthetic cathinones are spreading rapidly across the global market. Further investigations ought to include more synthetic cathinones, as well as different types of biological samples.

Maslina (Olea europaea L.) je jedna od glavnih poljoprivrednih kultura mediteranskog područja. Otkriveno je da su osim ulja i listovi masline bogat izvor komponenti s farmakološkim učinkom. U ovom radu analiziran je sastav eteričnog ulja i hidrolata u različitim razvojnim fazama masline. Vodenom destilacijom u aparaturi po Clevengeru iz nekoliko uzoraka listova masline izolirana su eterična ulja i hidrolati te identificirani GC/MS analizom. U prvom uzorku eteričnog ulja najzastupljeniji spoj bio je ß-ionon (20.4%), u drugom germakren D (31.2%), u trećem endo-fenhil acetat (12.7%), u četvrtom dokosan (40.1%), u petom n-dodekanol (30.6%) i u šestom kariofilen oksid (17.1%). U uzorcima hidrolata najzastupljeniji spoj u većini uzoraka bio je ß-ionon: u prvom uzorku u količini od 15.9%, u drugom uzorku u količini od 40.3%, u trećem uzorku u količini od 42.8%; u četvrtom uzorku najzastupljeniji spoj bio je biciklogermakren (39.5%), u petom ß-ionon (25.3%) i u šestom najzastupljeniji je bio miristicin (35%). Spojevi koji su izolirani u svim uzorcima listova, ili u eteričnom ulju ili hidrolatu su: α-pinen, ß-kariofilen, α-humulen, allo-aromadendren, ß-ionon, miristicin, palmitinska kiselina, oleinska kiselina te dokosan, trikosan i tetrakosan., Olive (Olea europaea L.) is one of the main agricultural crops of the Mediterranean area. It has been discovered that apart from oil, olive leaves are also a rich source of components with pharmacological effect. In this paper the composition of essential oils and hydrolates was observed in different life stages of olive. By aqueous distillation in Clevenger's apparatus, essential oils and hydrolates were isolated from several olive leaf samples and identified by GC/MS analysis. In the first sample of essential oil the most common compound was β-ionone (20.4%), in second germacrene D (31.2%), in third endo-fenchyl acetate (12.7%), in fourth docosane (40.1%), in fifth n-dodecanol (30.6 %) and in sixth caryophyllene oxide (17.1%). In hydrolates the most common compound in most of the samples was β-ionone: in first sample in the amount of 15.9%, in second sample in the amount of 40.3%, in third sample in the amount of 42.8%; in fourth sample the most common component was bicyclogermacrene (39.5%), in fifth ß-ionone (25.3%) and in sixth myristicin (35%). The compounds that were isolated from all of the samples, either from essential oil or hydrolate, were: α-pinene, ß-caryophyllene, α-humulene, allo-aromadendrene, ß-ionone, myristicin, palmitic acid, oleic acid and docosane, tricosane and tetracosane.

Eterična ulja nastaju kao specijalizirani metaboliti aromatičnih biljaka. Najčešće se dobivaju postupkom destilacije zbog svojstva hlapljivosti. To su uglavnom bistre i bezbojne tekućine. Gustoća im je najčešće manja od gustoće vode. Eterična ulja se danas najviše primjenjuju u kozmetologiji, za proizvodnju dermatokozmetičkih pripravaka i parfema, a zbog svog repelentnog djelovanja koriste se u različitim pripravcima za zaštitu od kukaca. Određena eterična ulja se primjenjuju u farmakologiji. Hidrolati su nusprodukti destilacije biljnog materijala pri ekstrakciji eteričnih ulja. Hidrolati se koriste u kozmetičke svrhe kao prirodni tonici ili kao vodena faza u izradi krema, gelova, emulzija i maski. Rod Salvia pripada porodici Lamiaceae koja ima veliki farmaceutsko–ekonomski značaj. Iz biljnog materijala vrsta Salvia officinalis L., Salvia sclarea L., Salvia bertolonii Vis. i Salvia verticillata L. izolirana su eterična ulja vodenom destilacijom u aparaturi po Clevenger – u. Dobiveni uzorci eteričnih ulja i hidrolata analizirani su sustavom plinske kromatografije – masene spektrometrije i plinske kromatografije – plameno-ionizacijske kromatografije. Rezultati su pokazali da postoje razlike u kvalitativnom i kvantitativnom sastavu eteričnih ulja istraživanih vrsta roda Salvia, te razlike u sastavu eteričnih ulja i hidrolata iste vrste., Essential oils are the specialized metabolites of aromatic herbs. The most common way of isolation is by the distillation process because of their volatility properties. They are generally clear and colorless liquids. Their density is usually smaller than the water density. Essential oils are mostly used in cosmetic industry, for the preparation of dermatocosmetics and perfumes, and are often used in the various insect protection formulations because of their repellent activity. Some essential oils are being used in pharmacology. Hydrosols are by-products of the distillation of herb material while extracting essential oils. They are used in cosmetic industry as natural tonics, or as a waters phase while preparing creams, gels, emulsions and masks. Genus Salvia belongs to the Lamiaceae family which has pharmaceutical-economic significance. From the herb material of Salvia officinalis L., Salvia sclarea L., Salvia bertolonii Vis. and Salvia verticillata L.., essential oils are isolated by the distillation in Clevenger apparatus. Samples of the essential oils and hydrosols are analysed by gas chromatography - mass spectrometry and gas chromatography - flame ionization chromatography. The results showed that there are differences in qualitative and quantitative composition of the essential oils from Salvia species and differences in composition of the essential oils and hydrosols from the same species.

Ciljevi istraživanja: Razviti metodu određivanja fenola plinskom kromatografijom s masenim detektorom, ispitati optimalne uvjete rada GC-MS-a pri kojima je moguća kvantifikacija fenola te odrediti koncentraciju fenola u biološkom uzorku mokraće. Mjesto istraživanja: Kemijsko-toksikološki laboratorij Kliničkog odjela za sudsku medicinu Zavoda za patologiju, sudsku medicinu i citologiju, KBC Split. Materijali i metode: Pripremljena su četiri miksa standardnih otopina postupnim razrjeđivanjem fenola s kloroformom. Odabrane su tri skupine instrumentalnih parametara (metoda 1, 2 i 3) kako bi se utvrdilo kojom metodom se dobije najbolji odziv signala na kromatogramu. U tri biološka uzorka mokraće dodan je proizvoljno određen volumen MIX-a 2. Uzorci su za analizu obrađeni ekstrakcijom na čvrstoj fazi, SPE, i analizirani na GC-MS-u. Rezultati: Provedenom analizom jednake koncentracije standarda najbolji odziv signala na detektoru ostvaren je metodom 3 s parametrima analize: volumen injektiranja:1 μl, temperatura injektora:250 °C, protok plina nosioca:1,54 ml/min i ukupno trajanje temperaturnog programa:10 minuta (60 °C 1 minutu, 10 °C/min do 170 °C). Analizom uzoraka mokraće uspješno je detektiran i kvantificiran fenol u dva od tri uzorka. Dobivena koncentracija fenola u uzorku 1 bila je 593,74 ng/ml, a u uzorku 2 1080 ng/ml. Zaključak: Odabranim instrumentalnim parametrima moguće je detektirati i kvantificirati fenol iz bioloških uzoraka mokraće. SPE je vrlo dobra tehnika predobrade uzorka, ali su potrebne dodatne analize da bi se utvrdila količina nečistoća koje mogu interferirati u analizi. Osim toga, potrebno je provesti dodatne analize kako bi se potvrdila primjenjivost same metode na realne biološke uzorke mokraće., Objectives: Objectives of this study were to develop a method for determination of phenol with gas chromatography-mass spectrometry, determine optimal parameters of the instrument and to quantify the phenol in three different biological samples of urine by using the selected method. Settings: LABORATORY OF TOXICOLOGY, DEPARTMENT OF PATHOLOGY, MEDICINE AND CYTOLOGY, University Hospital of Split. Materials and methods: Four mixes of standard solutions were prepared by gradually diluting phenol with chloroform. Three different groups of instrumental parameters were selected (method 1, 2 and 3) to determine which method gives the best signal on the chromatogram. A voluntary defined volume of MIX 2 was injected in three urine samples. The samples were prepared for the analysis by using solid phase extraction and analyzed with GC-MS method. Results: By analysing three equal concentrations of standard solution using all three methods, it was noticed that method 3 gives the best signal on the detector. Parameters of analysis for method 3 were: injection volume:1 μl , injector temperature:250 °C, carrier gas flow (helium):1,54 ml/min, program time:10 minutes (60 °C for 1 minute and 10 °C per minute til 170 °C). Two out of three urine samples were successfully detected and quantified with phenol. Sample 1 had the phenol concentration of 593,74 ng/ml and sample 2 1080 ng/ml. Conclusion: It is possible to detect and quantify the phenol from the biological samples of urine by using selected method 3. SPE is a good technique of sample preparation, but additional analysis are neccessary to establish the quantity of interferences that drop behind and can affect the analysis.It is also neccessary to carry out additional analysis on real biological samples to be able to confirm these techniques of sample preparation and analysis.

Ciljevi istraživanja: Cilj ove eksperimentalne studije bio je razviti GC-MS metodu za kvantitativno određivanje sintetskih kanabinoida JWH-018, JWH-019, JWH-073, JWH-210 i ADB-PINACA te razvijenu metodu potom primijeniti na kvantitativno određivanje navedenih sintetskih kanabinoida u biološkim uzorcima mokraće. Materijal i metode: Standardne otopine sintetskih kanabinoida, pripremljene razrijeđivanjem osnovnih standarda u metanolu, dodane su u biološki uzorak mokraće, dokazano negativan na prisustvo sredstava ovisnosti, kako bi se dobile umjerne krivulje analiziranih sintetskih kanabinoida. Koristeći nepoznate volumene tih standardnih otopina, pripremljena su dva biološka uzorka mokraće. Uzorci su pripremljeni za analizu ekstrakcijom tekuće-tekuće (LLE), a potom analizirani GC-MS metodom koja omogućuje istovremeno snimanje ukupnog ionskog kromatograma u području od 50-600 m/z vrijednosti i snimanje samo odabranih iona. Optimiran je i temperaturni program. Rezultati: ADB-PINACA, JWH-019 i JWH-210 potvrđeni su u oba analizirana uzorka, dok su JWH-073 i JWH-018 potvrđeni samo u uzorku 1, u koji je dodan veći volumen pripremljenih standardnih otopina. Masene koncentracije detektiranih sintetskih kanabinoida izračunate su pomoću prethodno izrađenih umjernih krivulja. Zaključci: Rezultati ovog istraživanja potvrdili su izbor GC-MS tehnike za kvantitativno određivanje sintetskih kanabinoida u biološkim uzorcima mokraće. Radi povećanja stabilnosti analiziranih spojeva, uzorke je potrebno prethodno derivatizirati. Zbog sve veće pojavnosti novih analoga, strukturno sličnih ishodišnim molekulama, potrebno je razvijati nove analitičke metode za identifikaciju sintetskih kanabinoida i njihovih metabolita u biološkim uzorcima., Objectives: Aim of this experimental study was to develop a GC-MS method for quantitative determination of synthetic cannabinoids JWH-018, JWH-019, JWH-073, JWH-210 and ADB-PINACA. Also, our objective was to quantitatively determine these synthetic cannabinoids in urine samples using the developed method. Materials and methods: Standard solutions of synthetic cannabinoids prepared by diluting original standards in methanol were added to the biological sample of urine, that tested negative for substances of abuse, to obtain calibration curves for analyzed synthetic cannabinoids. Using unknown volumes of standard solutions, two urine samples were prepared. The samples were prepared for analysis by liquid-liquid extraction (LLE) and then analyzed by a GC-MS method using mode that simultaneously records total ion chromatogram in the area of 50-600 m/z values and single ion monitoring scanning mode. The temperature program was also optimized. Results: ADB-PINACA, JWH-019 and JWH-210 were confirmed in both analyzed samples, while JWH-073 and JWH-018 were only confirmed in sample 1, to which a larger volume of prepared standard solutions was added. The mass concentrations of detected synthetic cannabinoids were calculated using previously prepared calibration curves. Conclusion: This study confirmed the GC-MS technique for quantitative determination of synthetic cannabinoids in biological samples of urine. In order to increase the stability of the analyzed compounds, it is necessary to include the derivatisation step prior to GC-MS analysis. Due to the increasing presence of new analogues, structurally similar to origin molecules, there is a need for development of analytical methods for the identification of synthetic cannabinoids and their metabolites in biological samples.

Ciljevi istraživanja: Kvalitativno dokazati prisutnost metilksantina u uzorcima čokolade i biološkim uzorcima mokraće primjenom GC-MS metode. Utvrditi koja je metoda, SPE ili LLE metoda, prikladnija. Usporediti rezultate analize dobivene nakon pripreme bioloških uzoraka LLE metodom kod različitih ispitanika. Materijali i metode: Korišteni su uzorci 11 čokolada (3 tamne i 8 mliječnih čokolada) te biološki uzorci urina tri ispitanika. Uzorci čokolada pripremljeni su SPE metodom, dok su Dorina čokolada za kuhanje te biološki uzorci pripremljeni LLE metodom. Svi uzorci su analizirani na GC-MS uređaju. Rezultati: U 10 uzoraka čokolade te u svim biološkim uzorcima detektirani su teobromin i kofein. Uzorci pripremljeni za analizu LLE metodom dali su bolji signal od uzoraka pripremljenih za analizu SPE metodom. Postoje razlike u signalima metilksantina kod različitih ispitanika. Zaključci: Analizom provedenom GC-MS tehnikom uspješno je kvalitativno dokazana prisutnost metilksantina u uzorcima 3 crne i 7 mliječnih čokolada te u biološkim uzorcima mokraće. LLE metoda pokazala je veću učinkovitost u pripremi uzoraka za analizu od SPE metode. Analizom provedenom GC-MS tehnikom uspoređeni su rezultati dobiveni nakon pripreme bioloških uzoraka ekstrakcijom tekuće-tekuće kod 3 različita ispitanika. Utvrđeno je kako postoje razlike u rezultatima te je potrebno provesti daljnja ispitivanja usporedbe bioloških uzoraka., Objectives: Qualitatively demonstrate the presence of methylxanthines in chocolate samples and biological samples of urine using the GC-MS method. Determine what method, SPE or LLE method, is more appropriate. Compare the results of the analysis obtained after the preparation of biological samples by the LLE method in different subjects. Materials and methods: Samples of 11 chocolates and biological samples of urine were used. Chocolate samples were prepared by the SPE method, while Dorina Chocolate for cooking and biological samples were prepared by the LLE method. All samples were analyzed with GC-MS method. Results: In 10 chocolate samples and in all biological samples, theobromine and caffeine were detected. Samples prepared for the LLE method analysis provided a better signal from samples prepared for SPE analysis. There are differences in the methylsantine signals in different subjects. Conclusion: The presence of methylxanthines in 3 black and 7 milk chocolate samples and in biological samples has been successfully demonstrated. LLE method showed greater efficiency in preparation of samples for analysis. It has been found that there are differences in results obtained after the preparation of biological samples by liquid-liquid extraction in 3 different subjects and a further study of the comparison of biological samples has to be carried out.

Ciljevi istraživanja: Kvalitativna analiza dječjih krema, usporedba dobivenih rezultata s deklaracijom proizvoda te pronalazak poveznice između cijene proizvoda i prisustva nepoželjnih sastojaka. Ustroj istraživanja: Eksperimentalna studija Mjesto istraživanja: Kemijsko-toksikološki laboratorij Kliničkog odjela za sudsku medicinu Zavoda za patologiju, sudsku medicinu i citologiju, KBC Split Materijali i metode: Ispitano je 10 uzoraka dječjih krema, raspoređenih u dva cjenovna ranga: 5 proizvoda s cijenom nižom i 5 s cijenom višom od 47,66 kn/100 mL. Za analitičku pripremu 0,1g uzorka ekstrahiran je smjesom otapala: kloroform, etilacetat i N-heksan (v/v/v = 1:1:1). Za usporedbu učinka otapala na ekstrakciju, uzorak br. 1 dodatno je otopljen u samom kloroformu. Kvalitativna analiza provedena je GC-MS metodom. Rezultati: Ispitivani nepoželjni sastojci su ftalati, parabeni, fenoksietanol, BHA i BHT, lanolin i parfemi. U 80% uzoraka detektiran je barem jedan od traženih nepoželjnih sastojaka dječjih krema, pri čemu u pet proizvoda koji pripadaju skupini nižeg te tri proizvoda koji pripadaju skupini višeg cjenovnog ranga. Odstupanje od deklaracije za detektirane nepoželjne sastojke zabilježeno je za dietilftalat i BHT, i to u skupini proizvoda nižeg cjenovnog ranga. Usporedbom kromatograma uzorka br. 1 pripremljenog na dva načina, prednost je dana smjesi otapala. Zaključak: Usporedbom cijene proizvoda u kojima su detektirani nepoželjni sastojci nisu dobiveni nedvojbeni rezultati. Utvrđena je povezanost cijene proizvoda i podudaranja detektiranih sastojaka s deklaracijom na ambalaži, odstupanja su prisutna samo u skupini nižeg cjenovnog ranga. Potrebna je provedba daljnjih ispitivanja u cilju detekcije iznimno niskih koncentracija nepoželjnih i nedeklariranih sastojaka., Objectives: Qualitative determination of ingredients in children skincare products, comparison of the results with the product declaration and finding a correlation between the price of the product and the presence of undesirable ingredients. Design: Experimental study Settings: Laboratory of toxicology, Department of pathology, medicine and cytology, University Hospital of Split Materials and methods: Ten samples of baby creams were analyzed and divided into two price ranges: 5 products with price lower and 5 products with price greater than 47.66 kn/100 mL. 0.1g of each sample was extracted with a mixture of solvents: chloroform, ethylacetate and N-hexane (v/v/v=1:1:1). In order to compare the results of different solvents, sample no.1 was dissolved in chloroform as well. Qualitative analysis was preformed by GC-MS method. Results: Undesirable ingredients investigated in this study are phthalates, parabens, phenoxyethanol, BHA and BHT, lanolin and perfume. In 80% of samples at least one of the tested ingredients was detected, with 5 products belonging to the lower and 3 products belonging to the higher price range group. The deviation from the declaration for these detected undesirable substances was recorded for diethylphthalate and BHT, only in the lower price range product group. By comparing the chromatograms of sample no.1 prepared in two ways, a mixture of solvents was preferred. Conclusion: Correlation between price of the product and presence of undesirable ingredients was not conclusive. Correlation between the price of the product and deviations from the product declaration is established, with deviations present only in the lower price range group. More thorough studies are required to detect extremely low concentrations of undesirable and undeclared ingredients.