Determination of volatile carboxylic acids (C1–C5i) and lactic acid in aqueous acid extracts of silage by high performance liquid chromatography

1984 ◽  
Vol 35 (11) ◽  
pp. 1178-1182 ◽  
Author(s):  
Andrea Canale ◽  
Maria E. Valente ◽  
Angelo Ciotti
Author(s):  
Ruben Ashotovich Pogosyan ◽  
Olga Vladimirovna Nesterova ◽  
Dmitry Olegovich Bokov ◽  
Irina Alexandrovna Samylina

Objective: Pomegranate (Punica granatum L.) is a broadly used plant possessing a wide range of medicinal properties. In this research, we have mainly focused on the investigation of phenolic compounds of pomegranate fruit pulp (PFP).Methods: Fresh fruits of “Çəhrayı Gülöyşə,” “Kizil-anor,” and pomegranate varietal mixture were used as samples. High-performance liquid chromatography-ultraviolet (HPLC-UV) analysis of phenol carboxylic acids was performed with metal column Kromasil® C18 (4.6×250 mm, particle size 5 μm) and the acetonitrile-water-concentrated acid phosphoric system (400:600:5) under isocratic elution conditions (flow rate of 0.5 ml/min). Detection was carried out using a UV detector “GILSTON” UV/Visible model 151 at a wavelength of 280 nm.Results and Discussion: As a result of our research, we proposed chromatographic conditions for the separation of phenolic compounds, the conditions for sample preparation of PFP. Procedure for determination of phenolic carboxylic acids total content in terms of gallic acid by HPLC-UV method was developed. According to the obtained data, the content of phenolic carboxylic acids should be at least 0.7%.Conclusion: Procedure for the quantitative determination of gallic acid using the HPLC-UV method was developed. This method which can be used in the standardization of new medicinal plant raw materials - PFP, as well as extract preparations based on it in the future.


Author(s):  
Ruben Ashotovich Pogosyan ◽  
Olga Vladimirovna Nesterova ◽  
Dmitry Olegovich Bokov ◽  
Irina Alexandrovna Samylina

Objective: Pomegranate (Punica granatum L.) is a broadly used plant possessing a wide range of medicinal properties. In this research, we have mainly focused on the investigation of phenolic compounds of pomegranate fruit pulp (PFP).Methods: Fresh fruits of “Çəhrayı Gülöyşə,” “Kizil-anor,” and pomegranate varietal mixture were used as samples. High-performance liquid chromatography-ultraviolet (HPLC-UV) analysis of phenol carboxylic acids was performed with metal column Kromasil® C18 (4.6×250 mm, particle size 5 μm) and the acetonitrile-water-concentrated acid phosphoric system (400:600:5) under isocratic elution conditions (flow rate of 0.5 ml/min). Detection was carried out using a UV detector “GILSTON” UV/Visible model 151 at a wavelength of 280 nm.Results and Discussion: As a result of our research, we proposed chromatographic conditions for the separation of phenolic compounds, the conditions for sample preparation of PFP. Procedure for determination of phenolic carboxylic acids total content in terms of gallic acid by HPLC-UV method was developed. According to the obtained data, the content of phenolic carboxylic acids should be at least 0.7%.Conclusion: Procedure for the quantitative determination of gallic acid using the HPLC-UV method was developed. This method which can be used in the standardization of new medicinal plant raw materials - PFP, as well as extract preparations based on it in the future.


2020 ◽  
Vol 16 (1) ◽  
pp. 10
Author(s):  
Devi Wulandari ◽  
Gusrizal Gusrizal ◽  
Titin Anita Zaharah

<p>Telah dilakukan optimasi dan validasi metode penentuan asam glikolat dan asam laktat dalam krim menggunakan kromatografi cair kinerja tinggi. Pemisahan asam glikolat dan asam laktat dilakukan pada kolom fasa balik C-8menggunakan fasa gerak asam ortofosfat 0,1% dengan pH 3,5 dan detektor <em>UV-Visible</em>. Standar asam glikolat dan asam laktat dibuat dengan melarutkannya menggunakan asam ortofosfat 0,1% pH 3,5. Hasil eksperimen menunjukkan bahwa pada rentang konsentrasi 25 – 400 μg/mL, asam glikolat dan asam laktat memiliki kurva yang linear dengan koefisien korelasi masing-masing 0,9997 dan 0,9999. Uji presisi untuk larutan standar berkonsentrasi 100 µg/mL menghasilkan simpangan baku relatif sebesar 1,49% untuk asam glikolat dan 1,72% untuk asam laktat. Metode yang telah dioptimasi memberikan akurasi yang baik yang ditunjukkan oleh nilai perolehan kembali dari pengukuran tiga <em>spiked sample</em> dengan konsentrasi berbeda (50, 100, dan 150 μg/mL). Nilai perolehan kembali untuk masing-masing konsentrasi <em>spiked sample</em> adalah 97,12% ± 0,69; 98,76% ± 0,43; 100,80% ± 0,29 untuk asam glikolat dan 97,58% ± 0,39; 96,20% ± 0,68; 98,00% ± 0,38 untuk asam laktat. Batas deteksi dan batas kuantisasi untuk asam glikolat adalah 0,05 dan 0,17 μg/mL, sedangkan untuk asam laktat adalah 1,40 dan 4,67 μg/mL. Nilai kekasaran metode untuk asam glikolat pada hari pertama dan hari kedua adalah 1,43% dan 1,67%, sedangkan untuk asam laktat adalah 1,67% dan 1,25%. Metode yang telah dioptimasi dan divalidasi berpotensi untuk digunakan secara spesifik pada penentuan kadar asam glikolat dan asam laktat dalam krim.</p><p><strong>Optimization and Validation of Determination Methods of Glycolic Acid and Lactic Acid in Cream Using High-Performance Liquid Chromatography.</strong> A high-performance liquid chromatography analytical method for the determination of glycolic acid and lactic acid in creams has been optimized and validated. The separation was performed in a reverse phase C–8 column with a mobile phase of 0.1%, orthophosphoric acid at pH 3.5, and UV-Visible detector. The standard of glycolic acid and lactic acid was dissolved in 0.1% orthophosphoric acid at pH 3.5. The experimental results showed that in the concentration range of 25–400 μg/mL, glycolic acid and lactic acid showed a linear curve with a correlation coefficient of 0.9997 and 0.9999, respectively. The precision test for standard solutions containing 100 µg/mL resulted in a relative standard deviation of 1.49% for glycolic acid and 1.72% for lactic acid. The optimized method provided good accuracy indicated by the recovery of the measurement of three spiked samples in different concentrations (50, 100, and 150 μg/mL). The recovery for each concentration of the spiked sample was 97.12% ± 0.69; 98.76% ± 0.43; 100.80% ± 0.29 for glycolic acid and 97.58% ± 0.39; 96.20% ± 0.68; 98.00% ± 0.38 for lactic acid. The limit of detection and limit of quantization for glycolic acid was 0.05 and 0.17 μg/mL, and for lactic acid was 1.40 and 4.67 μg/mL. The ruggedness of the method for glycolic acid on the first day and second day was 1.43% and 1.67%, while for lactic acid, it was 1.67% and 1.25%. The method that has been optimized and validated shows the potential to be used specifically for the determination of glycolic acid and lactic acid in the cream.</p>


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