An effective, simple and rapid analytical method using HPLC was developed for the analysis of monosodium glutamate (MSG) in various food samples obtained from local market in Turkey. The determination of MSG was performed by its derivatisation with o-phthaldialdehyde (OPA). A high-performance liquid chromatography-ultraviolet/diode array detection method was performed by using C 18 (150 mm 9 4.6 mm, 2.7 lm) column with the mobile phase consisting of 10 mM phosphate buffer solution (pH = 5.90) and methanol (75:25, v/v). The applied method was optimised and the validated. The method was linear from 1 to 50 lg mL À1 of MSG. The correlation coefficient value of the developed method was obtained as R 2 = 0.9999. The limit of detection and limit of quantification limits were 0.015 and 0.050 lg mL À1 , respectively. MSG contents of the food samples range from 0.09 g kg À1 to 120.80 g kg À1. The validated method was successfully applied for the analysis of MSG in several food samples.
In this study, an effective, simple and rapid high-performance liquid chromatography (HPLC) using fluorescence (FLD) method was developed and validated for the determination of monosodium glutamate (MSG) in 57 various food samples. Besides, HPLC-Evaporate Light Scattering Detection (ELSD) method was carried out for determination of MSG without derivatization. MSG analysis was performed by derivatization with dansyl chloride at excitation 328, emission 530nm with fluorescence detector. HPLC-FLD method was carried out by using C18 (150 mm, 4.6 mm, 2.7 μm) column with the mobile phase consisting of (Water: Methanol:Glacial Acetic Acid)/(54:45:1,v/v/v). The column temperature was set at 25°C and the flow rate was set at 0.5 mL min−1 with an injection volume 20 μL. The results were linear (R2 = 0.9999) with very low quantification limits. The applied method was optimized and the validated parameters such as LOD, LOQ, accuracy, precision, linearity and robustness were calculated. The obtained results were statistically compared with each other. The validated HPLC-FLD method was successfully applied for the analysis of MSG in all of the food samples. Moreover, HPLC-ELSD method was optimized and successfully demonstrated for detect the MSG without derivatization.
A novel analytical method, based on high-performance liquid chromatography with a UV (HPLC-UV) detection system for the sensitive detection of a genotoxic impurity (GTI) 5-amino-2-chloropyridine (5A2Cl) in a model active pharmaceutical ingredient (API) tenoxicam (TNX), has been developed and validated. The HPLC-UV method was used for the determination of GTI 5A2Cl in API TNX. The compounds were separated using a mobile phase composed of water (pH 3 adjusted with orthophosphoric acid): MeOH, (50:50: v/v) on a C18 column (150 × 4.6 mm i.d., 2.7 μm) at a flow rate of 0.7 mL min−1. Detection was carried out in the 254 nm wavelength. Column temperature was maintained at 40°C during the analyses and 10 μL volume was injected into the HPLC-UV system. The method was validated in the range of 1–40 μg mL−1. The obtained calibration curves for the GTI compound was found linear with equation, y = 40766x − 1125,6 (R2 = 0.999). The developed analytical method toward the target compounds was accurate, and the achieved limit of detection and limit of quantification values for the target compound 5A2Cl were 0.015 and 0.048 μg mL−1, respectively. The recovery values were calculated and found to be between 98.80 and 100.03%. The developed RP-HPLC-UV analytical method in this research is accurate, precise, rapid, simple and appropriate for the sensitive analysis of target GTI 5A2Cl in model API TNX.
Tarçın, bazı Cinnamomum (Lauraceae) türlerinin gövde kabuklarından elde edilen dünyanın en eski ve sık tüketilen baharatlarından biridir. 250'nin üzerinde Cinnamomum türünden kültüre alınan ve ticareti yapılanlar Cinnamomum verum (Seylan), C. cassia (Çin), C. burmanni (Endonezya) ve C. loureiroi (Vietnam)'dir. Toz edilmiş kabukların birbirlerinden ayrılması yalnızca anatomik, morfolojik, kromatografik ve spektroskobik yöntemler ile mümkündür. Tarçın ve uçucu yağı eşsiz aromasıyla gıda, kozmetik ve ilaç sanayiinde geniş kullanıma sahiptir. Son yıllarda tıbbi amaçlarla kullanılan, özellikle diyabet hastalarına önerilen tarçının bazı türleri antikoagülan ve hepatotoksik özellikte, "kumarin" bileşiğini yüksek miktarlarda taşımaktadır. Çalışmamızda ülkemizin çeşitli illerinde satışa sunulmuş 23 adet kabuk örneği anatomik-morfolojik olarak incelenmiş, bazı örneklerin uçucu yağ kompozisyonu Gaz Kromatografisi ve Gaz Kromatografisi/Kütle Spektrometresi sistemleri ile belirlenmiştir. Yüksek Performanslı Sıvı Kromatografisi ile tüm örneklerin taşıdıkları kumarin miktarı ortaya konmuştur. Ülkemiz piyasasından temin edilen 23 tarçın örneğinin 22'sinin "cassia tip" tarçın olduğu, kumarin miktarlarının 0.042 ile 12.8 mg/gr aralığında değiştiği saptanmıştır.
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