ANALISIS KADAR BETA KAROTEN DAN VITAMIN C BUAH JUWET (Syzigium cumini ) secara SPEKTROFOTOMETRI UV-VIS

Beta-carotene (?-Carotene) is an organic compound and is classified as a terpenoid. ?-Carotene is a red-orange pigment that is very abundant in plants and fruits. Beta-carotene is thought to have many functions that other compounds do not have (Subawati, 2009). The aim of this study was to determine ?-carotene levels in juwet fruit (Syzygium Cumini) by UV-Vis spectrophotometry. Juwet fruit samples (Syzygium Cumini) were extracted with acetone as a solvent. The extract obtained was extracted again with petroleum ether solvent, then saponified with 15% KOH solvent in methanol. The extract was liberated with distilled water. The extract obtained was dried over anhydrous Na2SO4. The extract obtained was analyzed qualitatively using Thin Layer Chromatography, and UV-Vis spectrophotometry at a wavelength of 332.1539 nm. The average level of ?-carotene in juwet fruit was 1.25 mg. Analysis of Vitamin C levels was carried out at a wavelength of 265.3 nm, the average level of Vitamin C in juwet fruit was 1.473

Multi-Target Analysis and Suspect Screening of Xenobiotics in Milk by UHPLC-HRMS/MS

The development of suspect or non-target screening methods to detect xenobiotics in biological fluids is essential to properly understand the exposome and assess its adverse health effects on humans. In order to fulfil that aim, the biomonitorization of human fluids is compulsory. However, these methods are not yet extensively developed, especially for polar organic xenobiotics in biofluids such as milk, as most works are only focused on certain analytes of interest. In this work, a multi-target analysis method to determine 245 diverse xenobiotics in milk by means of Ultra High Performance Liquid Chromatography (UHPLC)-qOrbitrap was developed. Under optimal conditions, liquid milk samples were extracted with acetonitrile in the presence of anhydrous Na2SO4 and NaCl, and the extracts were cleaned-up by protein precipitation at low temperature and Captiva Non-Drip (ND)—Lipids filters. The optimized method was validated at two concentration-levels (10 ng/g and 40 ng/g) obtaining satisfactory figures of merit for more than 200 compounds. The validated multi-target method was applied to several milk samples, including commercial and breast milk, provided by 4 healthy volunteers. Moreover, the method was extended to perform suspect analysis of more than 17,000 xenobiotics. All in all, several diverse xenobiotics were detected, highlighting food additives (benzothiazole) or phytoestrogens (genistein and genistin) in commercial milk samples, and stimulants (caffeine), plasticizers (phthalates), UV filters (benzophenone), or pharmaceuticals (orlistat) in breast milk samples.

DBU Catalysis: An Efficient Synthetic Strategy for 5,7-disubstituted-1,2,4- triazolo[1,5-a]pyrimidines

Aim and Objective: An efficient and facile DBU catalysed synthesis of highly significant motif 5,7-disubstituted-1,2,4-triazolo[1,5-a]pyrimidines under solvent-free condition has been reported. Materials and Methods: To a round bottom flask, 1.0 mmol of chalcone (1), 1.5 mmol of 3-amino-1,2,4- triazole (2) and 30 mol% of DBU were added at 70 °C and stirred in solvent-free condition. After the completion of the reaction (monitored by TLC), water (10 ml) was added. The aqueous layer was extracted with ethyl acetate (3 ×10 ml). The combined organic layers were dried over anhydrous Na2SO4. The combined organic layers were evaporated under reduced pressure and the resulting crude product was purified by column chromatography by using ethyl acetate and hexane as eluent. Results: Reaction using chalcone and 3-amino-1,2,4-triazole as model substrates were carried out under different reaction conditions and it was observed that 30 mol% of DBU under the solvent-free condition at 70 °C was the optimum temperature for the proposed synthesis. Conclusion: Use of DBU (an organocatalyst) as a base, operational simplicity, high yield of products and short reaction time are some of the significant advantages associated with the proposed strategy.

Komposisi kimia minyak atsiri daun cengkeh dari proses penyulingan uap

The chemical composition of clove leaf essential oil obtained from steam distillation process Essential oils are needed in various industries such as industrial perfumes, cosmetics, pharmaceuticals, food industry, and beverages. This study aims to determine the chemical composition of clove leaf essential oil from steam distillation process using GCMS. Dry clove leaves weighing 1.5 kg are included in the kettle flute and sealed properly. Steam from the boiler flows into the kettle with the pressure of 0.5 barG, 1 barG and 1.5 barG for 5, 6 and 7 hours. Mixture oil and water out of the condenser are accommodated and let stand for 24 hours to separate water and oil. Clove leaf oil was purified with 10% bentonite by weight of oil at a temperature of 50oC with stirring for 1 hour. Clove leaf oil that has separated from bentonite added anhydrous Na2SO4 and let stand for 15 minutes and then separate the water and Na2SO4 in oil. Samples with % yield of the largest in its chemical composition analysis using GCMS. Based on the results obtained the largest yield is 1.84% with content of eugenol is 65.03% and 20.94% trans-caryophyllene. Keywords : Clove leaf, Eugenol, Essential Oil, Steam distillationAbstrakMinyak atsiri sangat dibutuhkan dalam berbagai industri seperti industri parfum, kosmetik, farmasi, industri makanan, dan minuman. Penelitian ini bertujuan untuk mengetahui komposisi kimia minyak atsiri daun cengkeh dari proses penyulingan uap menggunakan analisa GCMS. Daun cengkeh kering seberat 1,5 kg yang sudah bersih dari kotoran dimasukkan dalam ketel suling dan ditutup dengan rapat. Steam dari boiler dialirkan ke ketel suling dengan tekanan 0,5 barG, 1 barG dan 1,5 barG selama 5, 6 dan 7 jam. Campuran minyak dan air yang keluar dari kondenser ditampung dan diamkan selama 24 jam untuk memisahkan air dan minyak. Minyak daun cengkeh dimurnikan dengan bentonit 10% dari berat minyak pada suhu 50oC sambil diaduk selama 1 jam. Minyak daun cengkeh yang telah terpisah dari bentonit ditambahkan Na2SO4 anhidrat dan diamkan selama 15 menit kemudian pisahkan air dan Na2SO4 dalam minyak. Sampel dengan % rendemen terbesar di analisa komposisi kimianya menggunakan GCMS. Berdasarkan hasil penelitian didapat rendemen terbesar adalah 1,84% dengan kadar yaitu eugenol 65,03% dan trans-caryophyllene 20.94%.Kata kunci : Daun cengkeh, Eugenol, Minyak atsiri, Penyulingan uap

MICROBIAL OXIDATION OF FINASTERIDE WITH MACROPHOMINA PHASEOLINA(KUCC 730)

Objectives: New microbial oxidative derivatives of Finasteride [17β-(N-tert-butylcarbamoyl)-4-aza-5α-androst-1-en-3-one] (1) has been investigated with Macrophomina phaseolina (ATCC730).Methods: Fermented media of Macrophomina phaseolina (ATCC730) was prepared to cultivate the fungal cultures . Substrate 1 was incubated in liquid media for 16 days. After sixteen days, filtration and extraction of the fermented media was carried out with 9 L DCM in three portions. Resulting organic extract was dried using anhydrous (Na2SO4), and evaporated to afford a brown gum (950 mg). This on chromatographic purification with MeOH in CH2Cl2 afforded the metabolites 2-4 . Results: Three oxidised metabolites of finasteride (1) which were identified as 15-oxo-finasteride (2), 11a-hydroxyfinasteride (3), and 15β-hydroxyfinasteride (4). Metabolite 2 was found to be new. The structure of the oxidised metabolites were elucidated by 1-D (1H, 13C) and 2-D NMR (COSY, HMBC, HMQC, NOESY) techniques and MS analyses.Conclusion: As a result of these study, oxidation at C-7, C-11 and C-15 positions were found. Metabolite 2 was identified as a new metabolite.

Gas Chromatographic Determination of Trifluralin, Diallate, Triallate, Atrazine, Barban, Diclofop-Methyl, and Benzoylprop-Ethyl in Sediments at Parts Per Billion Levels

A sensitive gas chromatographic method was developed for the multiresidue determination of 7 neutral herbicides in sediment. The sediment sample was ultrasonically extracted 3 times with acetone. The extract was concentrated to about 50 mL and then partitioned with 2% KHCO3 and CH2C12. The organic phase was dried over anhydrous Na2So4. The concentrated extract was then cleaned up on a 10% deactivated Florisil column, and the herbicides were separated into 2 fractions. Further cleanup of these fractions was performed on activated Florisil columns. Electron capture detection was used for analysis except for atrazine which was analyzed by nitrogen-phosphorus detection. Recoveries of the herbicides from fortified sediment samples at 3 levels were generally better than 80%. The practical detection limit of this method was 1 ppb or 1 ng/g based on a 50 g sediment sample.

Improved Rapid Colorimetric Method for Carbadox in Feeds

The extraction step in the rapid colorimetric method for determining carbadox in feeds was modified to include a water pretreatment for pelleted feeds. The extraction solvent was changed from dimethylformamide (DMF) to CHCl3-methanol (3+1). The water in the extract is removed with anhydrous Na2SO4, and an aliquot is evaporated to dryness, solubilized in DMF, and transferred to an alumina column. The method is then essentially the same as originally reported. Recoveries of carbadox added to unmedicated feeds were increased from 98 to 100% by inserting in the method the column recovery step to determine the standard absorbance values.

Optically active isomers of the genus Pinus and their application in chemosystematic

Aim. The aim of this work was the possibility of using the composition of essential oils enantiomers as chemomarkers for the genus Pinus. Methods. The plant materials were subjected to hydrodistillation in a Ginsburg type apparatus (0.2 kg each loading) for 1 h. The collected samples of essential oils were dried with anhydrous Na2SO4 and stored at 4.8℃ until analyzed. The enantioselective capillary GC analysis was conducted on a Cyclosil B capillary column (30 m x 0.32 mm, film thickness 0.25 μm, 30 % hepatkis (2,3-di-O-methyl-6-O-t-butyldimethylsilyl)-β-cyclodextrin in DB-1701). The relative amounts of individual components (in %) were calculated on the basis of GC peak areas without using correction factors. Results. The composition and enantiomeric terpene distribution of essential oils from the Pinus plants cultivated in the Central Botanical Gardens of Belarus is reported. Conclusions. The obtained experimental data indicate the presence of individual enantiomer composition features of essential oils of various representatives of the pine trees that can be used in chemosystematics of the genus Pinus. A common feature for the studied species of the genus Pinus is a significant predominance of (+)-Δ3-carene over (-)-form, the levorotatory isomer of β-pinene over (+)-form. As chemomarker for the section Cembra can be used enantiomeres excess (-)-limonene. Keywords: Pinus, essential oil, enantiomer, chemomarker.