Simultaneous Determination of Sildenafil and Tadalafil in Legal Drugs, Illicit/Counterfeit Drugs, and Wastewater Samples by High-Performance Liquid Chromatography

2016 ◽  
Vol 99 (4) ◽  
pp. 923-928 ◽  
Author(s):  
Ali Kemal Fidan ◽  
Sezgin Bakirdere
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Quantitative Measurement ◽  
Correlation Coefficients ◽  
Wastewater Sample ◽  
Counterfeit Drugs ◽  
Spiking Experiment ◽  
Wastewater Samples ◽  
Erectile Dysfunction Drug

Abstract A sensitive analytical method was developed for the simultaneous determination of sildenafil and tadalafil in legal drugs, illicit/counterfeit drugs, and wastewater samples. Chromatographic separation of two analytes was achieved on a C18 column with a mobile phase including 50 mM phosphate buffer at pH 6.0 and acetonitrile (35 + 65, v/v) at the flow rate of 1.0 mL/min. Analytes were separated from each other in 6 min with high resolution. LOD/LOQ values were calculated as 28/92 ng/mL for sildenafil citrate and 39/129 ng/mL for tadalafil. Calibration plots for both analytes were linear with correlation coefficients >0.9993. A validated method was successfully applied to legal and illicit erectile-dysfunction drug samples consumed in Istanbul, Turkey, and to wastewater samples. Nine different samples were analyzed for qualitative and quantitative measurement of their ingredients, and the results were compared with the values written on the labels of the drugs. The wastewater sample was also analyzed for its sildenafil and tadalafil content. To calculate the recoveries, a spiking experiment was performed and recovery rates for sildenafil and tadalafil were calculated as 101.30 ± 3.43 and 102.68 ± 1.59, respectively.

scholarly journals Simultaneous Determination of Clopidogrel and Pioglitazone by High Performance Liquid Chromatography in Bulk Drug and Dosage Forms

2013 ◽  
Vol 2 (1) ◽  
pp. 1-9 ◽  
Author(s):  
V Phani Kumar ◽  
Y Sunandamma
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Uv Detection ◽  
Isocratic Elution ◽  
Liquid Chromatographic Method ◽  
Bulk Drug ◽  
Liquid Chromatographic

A high performance liquid chromatographic method with UV detection was developed and validated for simultaneous determination of Pioglitazone and Clopidogrel. Separation was performed on a C18 column by isocratic elution with a mobile phase of Methanol: Acetonitrile: Water (80:10:10) at pH 4.6. The UV detection was set at 230 nm. The method proved to be specific, accurate, precise and linear over the concentration ranges of 20-120ppm for both Pioglitazone and Clopidogrel with correlation coefficients always >0.999 for both drugs. The intra-day and inter-day precision and accuracy were less than 2 for both analytes. DOI: http://dx.doi.org/10.3329/ijpls.v2i1.14580 International Journal of Pharmaceutical and Life Sciences Vol.2(1) 2013: 1-9

Simultaneous Determination of Cryptotanshinone, Tanshinone IA and Tanshinone IIA in Three Processing Products of White Flower S. Miltiorrhiza by HPLC

2012 ◽  
Vol 554-556 ◽  
pp. 2037-2040
Author(s):  
Yu Qin Li ◽  
Jing Zhao ◽  
Rui Duan ◽  
Bao Xiu Jia ◽  
Gui Rong You ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Salvia Miltiorrhiza ◽  
Correlation Coefficients ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
White Flower ◽  
Tanshinone Iia ◽  
Regression Equations

A reversed-phase high performance liquid chromatographic method was established for the simultaneous determination of tanshinones in three processing products of white flower Radix salvia miltiorrhiza. Cryptotanshinone, tanshinone IA and tanshinone IIA were successfully separated on a Yilite C18 column (250 mm x 4.6 mm, 5 µm). The mobile phase was a mixture of methanol, water, tetrahydrofuran and glacial acetic acid (70:24:5:1, v/v/v/v), employing isocratic elution at a flow rate of 1.0 mL/min. Detection was 254 nm. Regression equations revealed good linear relationship between the peak areas of the compounds and their concentrations (correlation coefficients: 0.9994 for cryptotanshinone, 0.9996 for tanshinone I A and 0.9996 for tanshinone IIA). The recoveries were between 98.03 % and 103.1 %. The method is simple, accurate and effective and can be used to determine the contents of tanshinones in processing products of Salvia miltiorrhiza bge. f. alba, and the contents of three tanshinones presented the stir-frying processing＜the crude drugs＜the wine prosessing.

scholarly journals Simultaneous Determination Of Sodium Benzoate And Sodium Cyclamate In Soft Drink Using High Performance Liquid Chromatography

2018 ◽  
Vol 3 (2) ◽  
pp. 62
Author(s):  
Ariya Wijaya Putra ◽  
Asri Darmawati ◽  
Juniar Mochtar
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Sodium Benzoate ◽  
High Performance ◽  
Soft Drink ◽  
Correlation Coefficients ◽  
Optimum Conditions ◽  
Sodium Cyclamate

Background: Sodium benzoate and sodium cyclamate are foods additives generally used as preservative and artificial sweeteners, respectively. Monitoring of sodium benzoate and sodium cyclamate need appropriate analytical method. Objective: The main objective of this study was to gain the optimum conditions for simultaneous determination of sodium benzoate and sodium cyclamate in soft drink by High Performance Liquid Chromatography. Methods: Measurement of the additives was performed in µ-Bondapak RP18 column using methanol:phosphate buffer of pH 4 (42:58) as mobile phase with flow rate of 1 mL/minute. Results: It has shown that correlation coefficients (r) of sodium benzoate and sodium cyclamate was 0.9997 and 0.9991 respectively. Recoveries of the two analyst were acceptable. Conclusions: Five out of nine samples tested contained sodium cyclamate higher than the recommended concentration. All sodium benzoate containing samples were within the recommended concentration.

A Rapid and Sensitive HPLC-FLD Method for the Determination of Retinol and Vitamin E Isomers in Human Serum

2019 ◽  
Vol 15 (7) ◽  
pp. 745-752
Author(s):  
Yi Yang ◽  
Dan Lu ◽  
Danni Yang ◽  
Shuo Yin ◽  
Jing Zhang ◽  
...  
Keyword(s):  
Vitamin E ◽  
Human Serum ◽  
Simultaneous Determination ◽  
Fluorescence Detection ◽  
High Performance ◽  
Correlation Coefficients ◽  
Serum Samples ◽  
Rapid Separation ◽  
Relative Standard

Background: Retinol and vitamin E are fat-soluble vitamins crucial for human health, yet their isomers’ distributions in the human body are still known roughly. In order to figure out the physical condition and evaluate the nutritional status of an individual, it is imperative to analyze retinol and VE isomers in human serum. Objective: This work aims to establish a rapid and simple high-performance liquid chromatography with fluorescence detection for simultaneous determination of retinol and vitamin E isomers in human serum. Methods: Separation was accomplished on a common C18 column thermostated at 25 oC, using a simple isocratic elution program of methanol/acetonitrile (85:15, v/v) at a flow rate of 1.0 mL/min. Fluorescence detection was operated using excitation/emission wavelengths of 329 nm/472 nm for retinol and 294 nm/338 nm for VE isomers, respectively. Results: Rapid separation was achieved within 13 min. Linear ranges of the method were 0.020-50.0 µg/mL, with correlation coefficients greater than 0.999. Detection limits and the quantification limits were 0.001-0.004 µg/mL and 0.003- 0.013 µg/mL, respectively. Mean recoveries were 84.1%- 98.2%, with intra-day and inter-day relative standard deviations less than 12.3% and 13.6%, respectively. This method has been applied to the simultaneous determination of retinol and 8 VE isomers in human serum samples with satisfactory results. Conclusion: A rapid, simple and robust method was developed for routine analysis of retinol and eight vitamin E isomers in human serum, providing a useful tool for clinical diagnosis and nutritional evaluation.

Simultaneous Determination of L-Ascorbic Acid and L-Ascorbylpalmitate Using RP-HPLC Method

2013 ◽  
Vol 716 ◽  
pp. 465-469
Author(s):  
Ye Lin Tian ◽  
Jun Kai Wang ◽  
Ping Sheng Leng ◽  
Yun Liu
Keyword(s):  
Ascorbic Acid ◽  
Simultaneous Determination ◽  
Methyl Palmitate ◽  
High Performance ◽  
Correlation Coefficients ◽  
Reversed Phase ◽  
Hplc Method ◽  
Enzymatic Transesterification ◽  
Rp Hplc

A rapid reversed phase highperformance liquid chromatography (RP-HPLC) method was developed for the simultaneous analysis of L-ascorbic acid and L-ascorbylpalmitate (AP). The chromatography was performed on a SSI model 2300-525 high performance liquid chromatographequipped with anAlltechApollo C18 column at 30 oC.The mobile phase was acetonitrile-water (90:10,v/v) with the flow rate of 1.0 mL/min. UV detection wavelength was 250 nm. This method permits the simultaneous determination of ascorbic acid and AP in the synthesis of AP transesterified with methyl palmitate and ascorbic acid. The detection limit of ascorbic acid and AP was 0.07μg/mL and 0.12μg/mL, respectively. The recovery was 90.59 ± 3.04% for ascorbic acid and 101.3 ± 4.81% for AP. The linearity range for ascorbic acid and AP was in the range of 0.1 - 0.7 mg/mL and 0.4 - 4.0 mg/mL, respectively. Correlation coefficients (R2) were 0.9910 for ascorbic acid and 0.9986 for AP. The proposed method could be used for routine quality control of AP synthesis with methyl palmitate and ascorbic acidby enzymatic transesterification.

Instrumental Determination of Energy Oxygen and BOD5

1992 ◽  
Vol 26 (5-6) ◽  
pp. 1345-1353 ◽  
Author(s):  
L. L. Ciaccio
Keyword(s):  
Microbial Population ◽  
Circulatory System ◽  
Weighted Average ◽  
Correlation Coefficients ◽  
Wastewater Sample ◽  
Excellent Correlation ◽  
Temperature Dependent ◽  
Microbiological Oxidation ◽  
Wastewater Samples

An instrument has been developed that measures the amount of oxygen consumption of a wastewater sample in the presence of excess microbial population and dissolved oxygen. In a closed circulatory system the sample experiences rapid microbiological oxidation with a measurement of oxygen consumed (designated EO, energy oxygen) by a DO electrode. The ABODA instrument (automatic BOD analyzer) measures EO of wastewater samples in less than one hour. EO shows an excellent correlation to BOD5 with correlation coefficients, r, of 0.997 and 0.99 for glucose-glutamate standard, and raw sewage and primary effluent samples, respectively. The reproduceability for the analyses are as follows: EO, 209 analyses with a weighted average cv of ± 5.1 % and BOD5, 200 analyses with a weighted average cv of ±9.8%. The instrumental determination of EO is not temperature dependent as the BOD5 test. Considering these factors the instrumental determination of EO allows the rapid measurement of BOD5.

scholarly journals Simultaneous Analysis of Ursolic Acid and Oleanolic Acid in Guava Leaves Using QuEChERS-Based Extraction Followed by High-Performance Liquid Chromatography

2017 ◽  
Vol 2017 ◽  
pp. 1-7 ◽  
Author(s):  
Chang Xu ◽  
Yiyi Liao ◽  
Chunyan Fang ◽  
Makoto Tsunoda ◽  
Yingxia Zhang ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Ursolic Acid ◽  
Oleanolic Acid ◽  
High Performance ◽  
Correlation Coefficients ◽  
Guava Leaves ◽  
Guava Leaf

In this paper, a novel method of QuEChERS-based extraction coupled with high-performance liquid chromatography has been developed for the simultaneous determination of ursolic acid (UA) and oleanolic acid (OA) in guava leaves. The QuEChERS-based extraction parameters, including the amount of added salt, vortex-assisted extraction time, and absorbent amount, and the chromatographic conditions were investigated for the analysis of UA and OA in guava leaves. Under the optimized conditions, the method showed good linearity over a range of 1–320 μg mL−1, with correlation coefficients above 0.999. The limits of detection of UA and OA were 0.18 and 0.36 μg mL−1, respectively. The intraday and interday precision were below 1.95 and 2.55%, respectively. The accuracies of the UA and OA determinations ranged from 97.4 to 111.4%. The contents of UA and OA in the guava leaf samples were 2.50 and 0.73 mg g−1, respectively. These results demonstrate that the developed method is applicable to the simultaneous determination of UA and OA in guava leaves.

scholarly journals Fast Simultaneous Determination of Eight Sudan Dyes in Chili Oil by Ultra-High-Performance Supercritical Fluid Chromatography

2019 ◽  
Vol 2019 ◽  
pp. 1-8 ◽  
Author(s):  
Yunjia Yang ◽  
Jing Zhang ◽  
Jie Yin ◽  
Yi Yang
Keyword(s):  
Simultaneous Determination ◽  
Supercritical Fluid ◽  
Supercritical Fluid Chromatography ◽  
High Performance ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Sudan Dyes ◽  
Relative Standard ◽  
Sudan Iv

A rapid and simple ultra-high-performance supercritical fluid chromatography (UHPSFC) with photodiode array (PDA) method was developed and validated for simultaneous determination of eight Sudan dyes in chili oil. In particular, a pair of isomer, Sudan red B and Sudan IV, was included in the analysis. After being diluted with dichloromethane, the analytes were separated on an Acquity UPC2 HSS C18 SB column with gradient elution using CO2 as the mobile phase and acetonitrile/methanol (v/v, 45/55, containing 0.1% formic acid) as the organic modifier. Analytes were quantified by external calibration curves over ranges of 0.5–50 mg/L, with correlation coefficients above 0.999. The method gave recoveries of the target compounds (spiked at levels of 1, 5, and 25 mg/kg) ranging from 82.6 to 108.3%, with intraday and interday relative standard deviations of less than 8.0% and 8.6%, respectively. The limits of detection (LODs) and the limits of quantification (LOQs) for eight dyes were from 0.10 to 0.30 mg/kg and 0.30–1.00 mg/kg, respectively. This method was applied for the analysis of chili oil samples collected from the supermarket in Beijing. This validated that the UHPSFC-PDA method provides a useful strategy for the simultaneous determination of Sudan dyes in chili oil for routine analysis.

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