Development of a SPE-HPLC-PDA Method for the Determination of Tetracyclines in Soils

2014 ◽  
Vol 675-677 ◽  
pp. 288-294 ◽  
Author(s):  
Bao Li Sun ◽  
Yi Wei Dong ◽  
Hong Shan ◽  
Jin Li Huang ◽  
Cheng Feng Tong
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Extraction Efficiency ◽  
Soil Samples ◽  
Hplc Separation ◽  
Buffer Solution ◽  
Soil Extracts ◽  
Relative Standard ◽  
Chromatographic Condition

A simple and rapid SPE-HPLC/PDA method has been developed for the quantitative determination of tetracyclines in soils. An ultrasonic extraction system for the soil samples was confirmed as a combination of a 1:2 ratio of EDTA-McIlvaine buffer solution with methanol by comparing the extraction efficiency of 4 solvents and optimising the combination ratio. The soil extracts were purified and concentrated by Oasis-MAX cartridge followed by HPLC separation and PDA detection. The optimal chromatographic condition effectively separated the object and interfering substance, which can improve the sensitivity of the instrument. The limits of detection were lower than 20 μg·kg-1, and the limits of quantification were no more than 60 μg·kg-1 for all compounds in the soil. The recoveries of tetracyclines peaked at levels of 50-500 μg·kg-1 and averaged at 62.1% to 108.9% with relative standard deviation values of less than 5%. This method was applied to analyse real soil samples from suburban Beijing farmland, and TC and OTC residues were detected in the soil.

scholarly journals UV Spectrophotometric Method Development and Validation of Fimasartan Drug and Its Tablet Formulation

1970 ◽  
Vol 7 (5) ◽  
pp. 25-29
Author(s):  
Kaushik S Agrawal ◽  
Lokesh R Gandhi ◽  
Nitin S. Bhajipale S Bhajipale3
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Relative Standard Deviation ◽  
Spectrophotometric Method ◽  
Method Development ◽  
Cost Effective ◽  
Tablet Formulation ◽  
Relative Standard ◽  
Bulk Drug

A novel, safe and sensitive method of Spectrophotometric estimation in UV - region has been developed for the assay of Fimasartan in its tablet formulation. The present study was undertaken to develop and validate a simple, accurate, precise, reproducible and cost effective UV spectrophotometric method for the estimation of Fimasartan bulk and pharmaceutical formulation. The method have been developed and validated for the assay of Fimasartan using Methanol as diluent. Absorption maximum (λmax) of the drug was found to be 240nm. The quantitative determination of the drug was carried out at 240nm. The method was shown linear in the mentioned concentrations having correlation coefficient R2 of 0.999. The recovery values for Fimasartan ranged from 98.74% to 99.23%.The Percent Relative Standard Deviation of interday and intraday was 0.85% and 0.75% respectively. All the parameters of the analysis were chosen according to the International Conference on Harmonisation guideline and validated statistically using Relative Standard Deviation and Percent Relative Standard Deviation. Hence, proposed method was precise, accurate and cost effective. This method could be applicable for quantitative determination of the bulk drug as well as dosage formulation.   KEY WORDS: 

Innovative NSAID dosage forms: lornoxicam suppositories and their standardization

2021 ◽  
pp. 71-76
Author(s):  
Viktoriya Viktorovna Skupchenko ◽  
Ekaterina Nikolaevna Mekhonoshina
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Relative Standard Deviation ◽  
Absorption Spectra ◽  
Dosage Forms ◽  
Uv Spectrophotometry ◽  
Relative Standard ◽  
Standard Solutions

The article presents the studies on the development of a method for the quantitative determination of lornoxime in suppositories using UV spectrophotometry. The optical densities of the test solutions were recorded at a wavelength of 375 nm. The absorption spectra of standard solutions of lornoxicam, as well as of tested solutions of suppositories were obtained. The relative standard deviation was 2.31%.

scholarly journals First derivative ATR-FTIR spectroscopic method as a green tool for the quantitative determination of diclofenac sodium tablets

F1000Research ◽  
2020 ◽  
Vol 9 ◽  
pp. 176
Author(s):  
Khairi M. S. Fahelelbom ◽  
Abdullah Saleh ◽  
Ramez Mansour ◽  
Sadik Sayed
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Ftir Spectroscopy ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Spectroscopic Method ◽  
First Derivative ◽  
Drug Concentrations ◽  
Relative Standard

Background: Attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy is a rapid quantitative method which has been applied for pharmaceutical analysis. This work describes the utility of first derivative ATR-FTIR spectroscopy in the quantitative determination of diclofenac sodium tablets. Methods: This analytical quantitative technique depends on a first derivative measurement of the area of infrared bands corresponding to the CO stretching range of 1550-1605 cm-1. The specificity, linearity, detection limits, precision and accuracy of the calibration curve, the infrared analysis and data manipulation were determined in order to validate the method. The statistical results were compared with other methods for the quantification of diclofenac sodium. Results: The excipients in the commercial tablet preparation did not interfere with the assay. Excellent linearity was found for the drug concentrations in the range 0.2 – 1.5 w/w %.  (r2= 0.9994). Precision of the method was assessed by the repeated analysis of diclofenac sodium tablets; the results obtained showed small standard deviation and relative standard deviation values, which indicates that the method is quite precise. The high percentage of recovery of diclofenac sodium tablets (99.81, 101.54 and 99.41%) demonstrate the compliance of the obtained recoveries with the pharmacopeial percent recovery. The small limit of detection and limit of quantification values (0.0528 and 0.1599 w/w %, respectively) obtained by this method indicate the high sensitivity of the method. Conclusions: First derivative ATR-FTIR spectroscopy showed high accuracy and precision, is considered as nondestructive, green, low cost and rapid, and can be applied easily for the pharmaceutical quantitative determination of diclofenac sodium tablet formulations.

Synthesis and Application of p-Carboxyarsenazo for Spectrophotometric Determination of Cu(II) in Environment Water

2013 ◽  
Vol 830 ◽  
pp. 298-301 ◽  
Author(s):  
Lin Gao ◽  
Yan Hua Li ◽  
Sheng Jie Chen ◽  
Fang Chen ◽  
Yuan Fang Zhang ◽  
...  
Keyword(s):  
Standard Deviation ◽  
Water Samples ◽  
Absorption Maximum ◽  
High Sensitivity ◽  
Molar Absorptivity ◽  
Buffer Solution ◽  
Relative Standard ◽  
Sensitivity And Selectivity ◽  
Color Reagent

p-Carboxyarsenazo (CASA) color reagent was synthesized by simple diazotization reaction, and the chromomeric reaction between CASA with Cu(Ⅱ) has been studied by spectrophotometry. In pH=4.6 NaAc-HAc buffer solution, Cu(Ⅱ) reacted with CASA to form a red complex and exhibits an absorption maximum at 614 nm, Beer’s law is obeyed for 0-160 μg/L of copper in solution, the apparent molar absorptivity obtained is 1.57×104 L/(mol.cm), and the relative standard deviation (R.S.D.) is 1.6%. The proposed method exhibited high sensitivity and selectivity for Cu(Ⅱ). The results obtained by this method in the determination of environment water samples were accurate, sensitive and repeatable

Dibenzoyl Methane—A New Coupling Agent for Nitrite Determination

1994 ◽  
Vol 77 (6) ◽  
pp. 1639-1646 ◽  
Author(s):  
K Shanthi ◽  
N Balasubramanian
Keyword(s):  
Standard Deviation ◽  
Nitrogen Dioxide ◽  
Relative Standard Deviation ◽  
Coupling Agent ◽  
Soil Samples ◽  
Relative Standard ◽  
Trapping Solution ◽  
Color System ◽  
Water And Soil Samples

Abstract Dibenzoyl methane is introduced as a new coupling agent for the determination of nitrogen dioxide in air and for nitrite in water and soil samples. Nitrogen dioxide is fixed as nitrite in NaOH–sodium arsenite trapping solution and also in triethanoamine trapping solution. The method is based on the diazo coupling reaction of p-nitro aniline with a new coupling agent, dibenzoyl methane. The azo dye formed under aqueous alkaline condition has an absorption maximum at 520 nm and obeys Beer’s law over a range of 0–20 μg nitrite per 10 ml analyte. The dye formed is stable for 40 h. The relative standard deviation is 2.8% for 10 determinations at 10 μg nitrite per 10 ml analyte. The color system upon extraction with isobutyl methyl ketone–amyl alcohol (1+1) shows a λ max at 520 nm and a Beer’s law range of 0–4 μg nitrite. The developed color is stable for 7 h in the organic phase. The relative standard deviation is 3.0% for 10 determinations at 2 μg nitrite. The molar extinction coefficient of the color system is 3.6 × 104 L/(mol·cm). The effect of interfering gases and ions on the determination is described. The method was applied to the determination of residual amounts of nitrogen dioxide present in the laboratory fume cupboard and in automobile exhaust gas. The method was also applied to the determination of nitrite and nitrate in water and soil samples. The results obtained were compared with the standard sulfanilamide–NEDA (N-1 naphthyl ethylene diamine dihydrochloride) method. The method can be used to determine levels as low as 0.5 μg nitrite in aqueous medium and 0.1 μg nitrite upon extraction.

scholarly journals First derivative ATR-FTIR spectroscopic method as a green tool for the quantitative determination of diclofenac sodium tablets

F1000Research ◽  
2020 ◽  
Vol 9 ◽  
pp. 176
Author(s):  
Khairi M. S. Fahelelbom ◽  
Abdullah Saleh ◽  
Ramez Mansour ◽  
Sadik Sayed
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Ftir Spectroscopy ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Spectroscopic Method ◽  
First Derivative ◽  
Drug Concentrations ◽  
Relative Standard

Background: Attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy is a rapid quantitative method which has been applied for pharmaceutical analysis. This work describes the utility of first derivative ATR-FTIR spectroscopy in the quantitative determination of diclofenac sodium tablets. Methods: This analytical quantitative technique depends on a first derivative measurement of the area of infrared bands corresponding to the CO stretching range of 1550-1605 cm-1. The specificity, linearity, detection limits, precision and accuracy of the calibration curve, the infrared analysis and data manipulation were determined in order to validate the method. The statistical results were compared with other methods for the quantification of diclofenac sodium. Results: The excipients in the commercial tablet preparation did not interfere with the assay. Excellent linearity was found for the drug concentrations in the range 0.2 – 1.5 w/w %.  (r2= 0.9994). Precision of the method was assessed by the repeated analysis of diclofenac sodium tablets; the results obtained showed small standard deviation and relative standard deviation values, which indicates that the method is quite precise. The high percentage of recovery of diclofenac sodium tablets (99.81, 101.54 and 99.41%) demonstrate the compliance of the obtained recoveries with the pharmacopeial percent recovery. The small limit of detection and limit of quantification values (0.0528 and 0.1599 w/w %, respectively) obtained by this method indicate the high sensitivity of the method. Conclusions: First derivative ATR-FTIR spectroscopy showed high accuracy and precision, is considered as nondestructive, green, low cost and rapid, and can be applied easily for the pharmaceutical quantitative determination of diclofenac sodium tablet formulations.

An Automated Procedure for the Determination of Ammonia in Tobacco

1972 ◽  
Vol 6 (4) ◽  
Author(s):  
P.F. Collins ◽  
W.W. Lawrence ◽  
J.F. Williams
Keyword(s):  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Distillation Method ◽  
Relative Standard ◽  
Tobacco Sample ◽  
Automated Determination

AbstractA procedure for the automated determination of ammonia in tobacco has been developed. Ammonia is extracted from the ground tobacco sample with water and is determined with a Technicon Auto Analyser system which employs separation of the ammonia through volatilization followed by colourimetry using the phenate-hypochlorite reaction. The procedure has been applied to a variety of tobaccos containing from 0.02 to 0.5 % ammonia with an overall relative standard deviation of 2 %. The accuracy of the procedure as judged by recovery tests and by comparison to a manual distillation method is considered adequate

scholarly journals Indirect and Direct Determination of the Casein Content of Milk by Kjeldahl Nitrogen Analysis: Collaborative Study

1998 ◽  
Vol 81 (4) ◽  
pp. 763-774 ◽  
Author(s):  
Joanna M Lynch ◽  
David M Barbano ◽  
J Richard Fleming
Keyword(s):  
Standard Deviation ◽  
Nitrogen Content ◽  
Relative Standard Deviation ◽  
Collaborative Study ◽  
Direct Determination ◽  
Raw Milk ◽  
Method Performance ◽  
Relative Standard ◽  
Milk Casein

Abstract The classic method for determination of milk casein is based on precipitation of casein at pH 4.6. Precipitated milk casein is removed by filtration and the nitrogen content of either the precipitate (direct casein method) or filtrate (noncasein nitrogen; NCN) is determined by Kjeldahl analysis. For the indirect casein method, milk total nitrogen (TN; Method 991.20) is also determined and casein is calculated as TN minus NCN. Ten laboratories tested 9 pairs of blind duplicate raw milk materials with a casein range of 2.42- 3.05℅ by both the direct and indirect casein methods. Statistical performance expressed in protein equivalents (nitrogen ⨯ 6.38) with invalid and outlier data removed was as follows: NCN method (wt%), mean = 0.762, sr = 0.010, SR = 0.016, repeatability relative standard deviation (RSDr) = 1.287℅, reproducibility relative standard deviation (RSDR) = 2.146%; indirect casein method (wt℅), mean = 2.585, repeatability = 0.015, reproducibility = 0.022, RSDr = 0.560℅, RSDR = 0.841; direct casein method (wt℅), mean = 2.575, sr = 0.015, sR = 0.025, RSDr = 0.597℅, RSDR = 0.988℅. Method performance was acceptable and comparable to similar Kjeldahl methods for determining nitrogen content of milk (Methods 991.20, 991.21,991.22, 991.23). The direct casein, indirect casein, and noncasein nitrogen methods have been adopted by AOAC INTERNATIONAL.

Quantitative Determination of some Carbonate Minerals in Greenschist Facies Meta-volcanic Rocks

1972 ◽  
Vol 9 (1) ◽  
pp. 36-42 ◽  
Author(s):  
Calvert C. Bristol
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Volcanic Rocks ◽  
Internal Standard ◽  
Greenschist Facies ◽  
Carbonate Mineral ◽  
Mineral Contents ◽  
X Ray ◽  
Fine Grained

X-ray powder diffraction methods, successful in quantitative determination of silicate minerals in fine-grained rocks, have been applied to the determination of calcite, dolomite, and magnesite in greenschist facies meta-volcanic rocks. Internal standard graphs employing two standards (NaCl and Mo) have been determined.Carbonate mineral modes (calcite and dolomite) for 6 greenschist facies meta-volcanic rocks obtained by the X-ray powder method have been compared to normative carbonate mineral contents calculated for the same rocks. This comparison showed a maximum variation of 7.7 wt.% between the X-ray modes and the normative carbonate mineral contents of the rocks. Maximum standard deviation for the X-ray modes of these rocks was equivalent to 4.4 wt.%.

Determination of Nitrate in Water by HPLC

2013 ◽  
Vol 448-453 ◽  
pp. 406-408
Author(s):  
Jing Liu ◽  
Xiao Na Ji ◽  
Qing Kai Ren ◽  
Sheng Shu Ai ◽  
Li Jun Wan ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Relative Standard Deviation ◽  
Recovery Rate ◽  
High Performance ◽  
Separation Efficiency ◽  
Fast Analysis ◽  
Relative Standard

We established a method fordetermination of nitrate in water by High Performance Liquid Chromatography(HPLC). The sample was analysed by HPLC-ADA and was quantitated by externalstandard method after being simply processed. This methd has the advantages ofhigh separation efficiency and fast analysis. The experiment result showed thatthe linearly dependent coefficient was0.994, the recovery rate was between 98.7%～105.7%,the relative standard deviation（RSD）wasless than 2.1 %, and the lowest detectable limit is 0.01ng (S/N=1.6).

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