PENGARUH REGENERASI KOLOM ALUMINA ASAM TERHADAP RECOVERY DAN KUALITAS 99mTc HASIL EKSTRAKSI PELARUT MEK DARI 99Mo HASIL AKTIVASI NEUTRON

PENGARUH REGENERASI KOLOM ALUMINA ASAM TERHADAP RECOVERY DAN KUALITAS 99mTc HASIL EKSTRAKSI PELARUT MEK DARI 99Mo HASIL AKTIVASI NEUTRON. Melalui kerjasama antara PTRR-BATAN, Chiyoda dan JAEA Jepang telah dilakukan pemurnian 99mTc dari 99Mo hasil aktivasi neutron dengan menggunakan metode kromatografi kolom alumina asam terhadap hasil ekstraksi MEK (Metil Etil Keton). Pemurnian 99mTc dengan metode kolom alumina asam hanya dapat digunakan satu kali dan pemurnian berikutnya harus diganti dengan kolom baru. Hal ini dinilai kurang praktis dan juga memerlukan biaya yang mahal. Dalam penelitian ini dicoba penggunaan kolom alumina asam untuk pemurnian 99mTc lebih dari satu kali dengan melakukan proses regenerasi dengan cara melewatkan larutan HNO3 0,1N setiap kali proses pemurnian selesai. Penelitian ini bertujuan untuk mendapatkan larutan 99mTc yang dapat digunakan untuk penandaan kit radiofarmaka. Parameter yang diamati dalam penelitian ini adalah recovery, profil elusi, pH, kemurnian radiokimia dan kemurnian radionuklida (lolosan 99Mo). Hasil penelitian yang dilakukan selama 5 hari telah diperoleh pH ~5, recovery > 60 %, kemurnian radiokimia > 95 % dan lolosan 99Mo tidak terdeteksi. Dari hasil perlakuan terhadap kolom alumina asam dengan larutan HNO3 0,1 N disimpulkan bahwa kolom alumina asam tidak perlu diganti setiap hari.Kata kunci: 99mTc, 99Mo, MEK, kolom alumina asam, kemurnian radiokimia. Purification of 99mTc from 99Mo activation using acidic alumina column chromatography system from MEK (Methyl Ethyl Keton) extraction has been carried out through cooperation between PTRR - BATAN, Chiyoda and JAEA Japan. This method has a limitation that acidic alumina column for purification of 99mTc can be used only once, for the next purification acidic alumina column should be replaced with new column, so it is less practical and also requires high cost. This study aims to obtain a 99mTc solution can be use for labelling of a radiopharmaceutical kit. In this study, the used of acidic alumina column for 99mTc purification was tried more than once by regeneration using 0.1N HNO3 solution after purification process is completed. Parameters observed in this study are the percent recovery, elution profile, pH, radiochemical purity and radionuclida purity. The results of observational studies conducted over 5 days has been obtained pH ~ 5,% recovery > 60%, radiochemical purity of > 95% and 99Mo leakage not detected. The treatment of acidic alumina column with 0,1 N HNO3 solution concluded that acidic alumina column does not need to be replaced every day.Keywords: 99mTc, 99Mo, MEK, acidic alumina column, radiochemical purity.

Liquid Chromatographic Determination of the Herbicide Isoxaben and Its Soil Metabolite in Soil and Soil-Turf Samples

A method Is described for the determination of residues of isoxaben and its principal soil metabolite In soil and soil-turf samples. Both compounds are extracted from samples by refluxing with methanol-water. An aliquot of the extract Is partitioned Into dichloromethane and purified by alumina column chromatography. Separate fractions containing isoxaben and metabolite are collected and subjected to liquid chromatography at conditions that are optimized for each compound. The detection limit for both compounds is 0.005 ppm. Residue identities are confirmed by chromatography on a different LC system.

Liquid Chromatographic Determination of Sulfamoyldapsone in Swine Tissues

A liquid chromatographic (LC) method is described for the quantitative determination of sulfamoyldapsone (2-sulfamoyl-4,4'-diaminodiphenyl sulfone) in swine muscle, liver, kidney, and fat. Sulfamoyldapsone was extracted from tissues with acetonitrile saturated with n-hexane. The extract was washed with n-hexane saturated with acetonitrile, concentrated, and cleaned up by alumina column chromatography. Sulfamoyldapsone was separated on an ODS column by using acetonitrile-methanol-water (6 + 18 + 76) and was detected at 292 nm. Overall average recovery of sulfamoyldapsone added to tissues at levels of 0.1 and 0.5 /μg/g was 93.3% ± 6.0. Detection limit was 0.02 μg/g in these tissues.

Determination of Olaquindox Residues in Swine Tissues by Liquid Chromatography

A liquid chromatographic (LC) method is described for determination of olaquindox residues in swine tissues. The drug is extracted from tissues with acetonitrile, and the extract is evaporated to dryness. This residue is cleaned up by alumina column chromatography. LC analysis is carried out on a Nucleosil C18 column, and olaquindox is quantitated by ultraviolet detection at 350 nm. The average recoveries of olaquindox added to tissues at levels of 0.2, 0.1, and 0.05 ppm were 74.0, 68.6, and 66.3%, respectively. The detection limit was 2 ng for olaquindox standard and 0.02 ppm in tissues.

Liquid Chromatographic Determination of Amprolium in Chicken Tissues, Using Post-Column Reaction and Fluorometric Detection

A method is presented for determination of amprolium residues in chicken muscles by a liquid chromatographic post-column reaction system. The drug is extracted from muscles with methanol, and the extract is concentrated to 3-4 mL. This aqueous solution is rinsed with n-hexane and cleaned up by alumina column chromatography. The drug is separated from the interferences on a LiChrosorb RP-8 column, reacted with ferricyanide in alkaline solution, and quantitated by fluorometric detection at 367 nm (excitation) and 470 nm (emission). Recoveries of amprolium added to chicken muscles at levels of 0.1 and 0.2 ppm were 74.9 and 80.9%, respectively. The detection limit was 1 ng for amprolium standard and 0.01 ppm in chicken muscles.

Deoxynivalenol in Winter Wheat: Thin Layer Chromatographic Method and Survey

A rapid method for the determination of deoxynivalenol (DON) in wheat was used to analyze 57 wheat samples collected from 4 midwestern states where the winter wheat crop was contaminated with Fusaria. The method involves sample extraction with acetonitrilewater (84 + 16), cleanup by charcoal-alumina column chromatography, and determination by thin layer chromatography (TLC), using an AlClj solution spray and heat to form a fluorescent derivative. Recoveries of DON added to wheat at levels as low as 0.2 μg/g averaged >80%. DON was detected at an average level of 3.6 μg/g; the levels ranged from 0.2 to 9.0 μg/g in 54 of 57 of the wheat samples. The quantity of DON was, in general, proportional to the percentage of total damaged kernels (grade). The chemical identity of DON was confirmed by mass spectrometry after isolation with preparative TLC.