scholarly journals KOMPONEN KIMIA ORGANIK LIMA JENIS ASAP CAIR

2021 ◽  
Vol 39 (1) ◽  
pp. 39-54
Author(s):  
Nur Adi Saputra ◽  
Sri Komarayati ◽  
, Gusmailina Gusmailina
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Theobroma Cacao ◽  
High Performance ◽  
Persea Americana ◽  
Schima Wallichii

Beberapa tanaman seperti kakao (Theobroma cacao), alpukat (Persea americana), puspa (Schima wallichii), sengon (Falcataria mollucana) dan tarik angin (Usnea sp.) banyak ditanam di masyarakat untuk kebutuhan buah-buahan atau kayu. Secara periodik, masyarakat memanen jenis-jenis tersebut untuk dimanfaatkan kayunya atau peremajaan tanaman. Pada umumnya, sortimen kayu digunakan untuk konstruksi sederhana, atau dibakar. Selain teknik pembakaran konvensional untuk menghasilkan arang, ada produk lain yang dapat dihasilkan yaitu asap cair menggunakan teknik pembakaran dengan menambahkan kondensor untuk menghasilkan asap cair. Asap cair memiliki kandungan kimia organik dengan beragam manfaat. Studi ini bertujuan untuk menganalisis kandungan kimia organik jenis asap cair dari jenis kayu kakao, kayu alpukat, kayu puspa, kayu sengon dan kayu tarik angin. Kelima jenis material studi dikarbonisasi menggunakan reaktor pirolisis pada suhu 400°C. Asap cair didapat dengan cara kondensasi uap karbonisasi kelima jenis tersebut. Analisis kandungan kimia organik asap cair menggunakan kromatografi gas-spektrometer massa (Gas Chromatography Mass Spektophotometry, GCMS) Pirolisys Type QP2010 dan High Performance Liquid Chromatography (HPLC). Analisis GCMS menunjukkan bahwa asap cair kayu kakao memiliki konsentrasi kelompok asam tertinggi, yaitu 45,53%, sementara konsentrasi asam asetatnya adalah 31,81%. Kehadiran kelompok fenol tertinggi terdapat pada asap cair kayu alpukat sebanyak 56,86%, di mana konsentrasi senyawa fenol mencapai 41,92%. Kelompok asam dan fenol merupakan jenis senyawa yang terkandung pada asap cair dan memiliki manfaat yang luas.

Determination of Impurities in Perampanel Bulk Drugs by High-Performance Liquid Chromatography and Gas Chromatography

2020 ◽  
Vol 16 ◽  
Author(s):  
Yun-Yan Xia ◽  
Qiao-Gen Zou ◽  
Yu-Fei Yang ◽  
Qian Sun ◽  
Cheng-Qun Han
Keyword(s):  
Gas Chromatography ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Quantitative Detection ◽  
Dihydrogen Phosphate ◽  
Phosphate Solution ◽  
Related Impurities ◽  
Bulk Drug

Background: High-performance liquid chromatography (HPLC) method has been used to detect related impurities of perampanel. However, the detection of impurities is incomplete, and the limits of quantification and detection are high. A sensitive, reliable method is in badly to be developed and applied for impurity detection of perampanel bulk drug. Objective: Methodologies utilising HPLC and gas chromatography (GC) were established and validated for quantitative determination of perampanel and its related impurities (a total of 10 impurities including 2 genotoxic impurities). Methods: The separation was achieved on a Dikma Diamonsil C18 column (250 mm × 4.6 mm, 5 μm) with the mobile phase of 0.01 mol/L potassium dihydrogen phosphate solution (A) and acetonitrile (B) in gradient elution mode. The compound 2-bromopropane was determined on an Agilent DB-624 column (0.32 mm × 30 m, 1.8 μm) by electron capture detector (μ-ECD) with split injection ratio of 1:5 and proper gradient temperature program. Result: Both HPLC and GC methods were established and validated to be sensitive, accurate and robust according to International Council for Harmonization (ICH) guidelines. The methods developed were linear in the selected concentration range (R 2≥0.9944). The average recovery of all impurities was between 92.6% and 103.3%. The possible production mechanism of impurities during the synthesis and degradation processes of perampanel bulk drug was also discussed. Five impurities were analyzed by liquid chromatography–mass spectrometry (LC-MS). Moreover, two of them were simultaneously characterized by LC-MS, IR and NMR. Conclusion: The HPLC and GC methods were developed and optimized, which could be applied for quantitative detection of the impurities, and further stability study of perampanel.

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