scholarly journals Investigation of linearity, detection limit (LD) and quantitation limit(LQ) of active substance from pharmaceutical tablets

2019 ◽  
Vol 70 (1) ◽  
pp. 259-262
Author(s):  
Afrodita Doina Marculescu ◽  
Cristian-Catalin Gavat ◽  
Aurel Nechita ◽  
Gabi Topor ◽  
Leonard Vasile Vasilescu ◽  
...  

The aim of this research was to exactly quantify pure sodium metamizole from tablets , using a spectrophotometric analysis in Visible range. The method applied has been subjected to a validation protocal which consisted in analyzing the following parameters: linearity of the method, detection limit (LD) , quantitation limit (LQ). Following actual dosing, pure sodium metamizole amount in tablet of pharmaceutical was found to be 477.477 mg assigned to a percentage content of 95.495 %, very close to official declared amount (500 mg), with an maximum average percentage deviation of only 4.505 % from the official declared active substance content. This value was situated below the maximum admissible percentage deviation from stated active substance content (� 5%), established by Romanian Pharmacopoeia, X-th Edition rules.

2019 ◽  
Vol 70 (2) ◽  
pp. 475-482
Author(s):  
Cristian Catalin Gavat ◽  
Leonard Vasile Vasilescu ◽  
Afrodita Doina Marculescu

The aim of this research was to exactly quantify pure sodium metamizole from tablets , using a spectrophotometric analysis in Visible range. The method applied has been subjected to a validation protocal which consisted in analyzing the following parameters: linearity of the method, detection limit (LD) , quantitation limit (LQ), Sandell�s sensitivity, interference of excipients, stability of prepared solutions, method and system precision, accuracy of the method. Following actual dosing, pure sodium metamizole amount in tablet of pharmaceutical was found to be 477.477 mg assigned to a percentage content of 95.495 %, very close to official declared amount (500 mg), with an maximum average percentage deviation of only 4.505 % from the official declared active substance content. This value was situated below the maximum admissible percentage deviation from stated active substance content (� 5%), established by Romanian Pharmacopoeia, X-th Edition rules.


2013 ◽  
Vol 12 (7) ◽  
pp. 460-465
Author(s):  
Sameer Amereih ◽  
Zaher Barghouthi ◽  
Lamees Majjiad

A sensitive colorimetric determination of fluoride in drinking water has been developed using a polymeric zirconium complex of 5-(2-Carboxyphenylazo)-8-Hydroxyquinoline as fluoride reagents. The method allowed a reliable determination of fluoride in range of (0.0-1.5) mg L-1. The molar absorptivity of the complex formation is 7695 ± 27 L mol-1 cm-1 at 460 nm. The sensitivity, detection limit, quantitation limit, and percentage recovery for 1.0 mg L-1 fluoride for the proposed method were found to be 0.353 ± 0.013 μg mL-1, 0.1 mg L-1, 0.3 mg L-1, and 101.7 ± 4.1, respectively.


2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Bei Zhou ◽  
Zongzhi Li ◽  
Shengrui Zhang

A hit-and-run (HR) crash occurs when the driver of the offending vehicle flees the crash scene without reporting it or aiding the victims. The current study aimed at contributing to existing literatures by comparing factors which might affect the crash severity in HR and non-hit-and-run (NHR) crashes. The data was extracted from the police-reported crash data from September 2017 to August 2018 within the City of Chicago. Two multinomial logistic regression models were established for the HR and NHR crash data, respectively. The odds ratio (OR) of each variable was used to quantify the impact of this variable on the crash severity. In both models, the property damage only (PDO) crash was selected as the reference group, and the injury and fatal crash were chosen as the comparison group. When the injury crash was taken as the comparison group, it was found that 12 variables contributed to the crash severities in both HR and NHR model. The average percentage deviation of OR for these 12 variables was 34%, indicating that compared with property damage, HR crashes were 34% more likely to result in injuries than NHR crashes on average. When fatal crashes were chosen as the comparison group, 2 variables were found to be statistically significant in both the HR and the NHR model. The average percentage deviation of OR for these 2 variables was 127%, indicating that compared with property damage, HR crashes were 127% more likely to result in fatalities than NHR crashes on average.


2016 ◽  
Vol 11 (2) ◽  
pp. 188 ◽  
Author(s):  
Bambang Wispriyono ◽  
Eko Handoyo

<p>Efek negatif dari polusi udara terhadap kesehatan manusia banyak diteliti termasuk polusi akibat sistem transportasi. Emisi kendaraan bermotor menghasilkan Benzena, Toluena dan Xylena (BTX) yang merupakan bahan kimia yang bersifat karsinogenik dan petugas pintu tol merupakan kelompok berisiko terpajan BTX. Penelitian bertujuan mengetahui risiko kesehatan akibat pajanan BTX pada petugas pintu tol. Desain penelitian adalah <em>cross-sectional</em> dengan pendekatan Analisis Risiko Kesehatan Lingkungan (ARKL) dan  faktor-faktor antropometri. Hasil penelitian menunjukkan pada pintu tol rata-rata konsentrasi (mean<span style="text-decoration: underline;">+</span>SD) benzena sebesar 0,00167<span style="text-decoration: underline;">+</span>0,000056 mg/m<sup>3</sup>, toluena sebesar 0,00124<span style="text-decoration: underline;">+</span>0.000049 mg/m<sup>3</sup> dan xylena sebesar 0,00147<span style="text-decoration: underline;">+</span>0,000063 mg/m<sup>3</sup> sedangkan pada kantor administrasi konsentrasi tidak terdeteksi oleh alat (<em>Method Detection Limit</em>). Rata-rata risiko non karsinogenik (RQ) BTX pada petugas pintu tol lebih tinggi secara signifikan dibandingkan dengan rata-rata RQ BTX petugas administrasi. Risiko kesehatan non karsinogenik dan karsinogenik belum menunjukkan adanya risiko kesehatan yang signifikan. Upaya pencegahan berupa pengelolaan manajemen risiko untuk pengendalian risiko bahan berbahaya di lingkungan perlu ditingkatkan.</p><p> </p><p><strong>Kata Kunci:</strong> Pintu Tol, Benzena, Toulena, Xylena</p><p> </p><p>The researches of BTX (Benzene, Toluene and Xylene) related to the health impacts have been done and published in any publications. One of the risk groups is toll gate’s workers who have been exposed every day with BTX. The design of this study is cross-sectional with Environmental Health Risk Analysis to determine the magnitude of health risks of BTX on the toll gate. The results showed at the toll workers’s respondents have  benzene concentration 0.00167+0.000056 mg/m<sup>3</sup>, toluene 0.00124+0.000049 mg/m<sup>3</sup> and xylene 0.00147+0,000063 mg/m<sup>3</sup> respectively, while in the administrative office’s respondents, BTX was undetectable (Minimum Detection Limit). The average RQ of toll gate respondents was significantly higher than administrative office’s respondents. In conclusion, the risk of all workers have the RQ ≤ 1. Non carcinogenic and carcinogenic health risks to all toll gate’s workers recently have not shown any risk yet. Nevertheless, risk management system should be developed and improved.</p><p> </p><p><strong>Keywords</strong>: Toll Gate, Benzene, Toulene, Xylene</p>


Author(s):  
KANCHARLA VIJAYALAKSHMI ◽  
BETHAPUDI SAMUEL ANAND ANDREWS ◽  
BOLINENI NAGESWARA RAO

Objective: We have developed a “stability-indicating RP-HPLC” procedure for the Bilastine (BLS) and montelukast (MTL) analysis of tablets. Methods: The quantification of BLS and MTL combination was implemented utilising a Waters column (C18, 5 μm, 250 mm and 4.6 mm). Isocratic mobile phase had 60% volume KH2PO4 of 0.1M strength with pH 4.2 units and 40% volume methanol at a flow with 1.0 ml/min speed. UV detection at 232 nm was done to examine BLS and MTL. Stability experiments of BLS and MTL under distinctive environments of stress were also performed. Results: The BLS and MTL were eluted at 1.810 min and 2.551 min, respectively. The responses were found to be linear for the concentration ranges of 10-30 µg/ml (BLS) and 5-15 µg/ml (MTL). Percent comparative standard deviance for precision was 0.331% (BLS) and 0.486% (MTL). Percent assay for accuracy was 98.96% (BLS) and 99.00% (MTL). The detection limit and quantitation limit measures for BLS were 0.018 µg/ml and 0.059 µg/ml, respectively, while for MTL it was 0.024 µg/ml and 0.081 µg/ml, respectively. Robustness studies authorized that the method is robust with percent comparative standard deviance of a highest 1.950%. Conclusion: The developed “stability-indicating RP-HPLC” procedure for the BLS and MTL analysis is simple, sensitive, precise, specific and robust, making it appropriate to the assessment of BLS and MTL in a tablet formulation.


2010 ◽  
Vol 7 (1) ◽  
pp. 704-712
Author(s):  
Baghdad Science Journal

Simple, rapid and sensitive spectrophotometric method was proposed for the analysis of metoclopramide hydrochloride (MPH) in pure form as well as in pharmaceutical tablets. The method is based on the diazotization reaction of MPH with sodium nitrite in hydrochloric acid medium to form diazonium salt, which is coupled with 1-naphthol in sodium hydroxide medium to form azo dye, showing absorption maxima at 550 nm. Beer’s law is obeyed in the concentration range of 0.4 – 18 µg mL-1 of MPH with detection limit 0.5448 µg mL-1. The molar absorptivity and Sandell’s sensitivity are 3.4969 × 104 L mol-1 cm-1 and 0.0101 µg cm-2, respectively. The method was successfully applied to the determination of MPH in pharmaceutical tablets without any interference from common excipients used as additives in tablets. The results agree favorably with the official British Pharmacopoeia method.


1994 ◽  
Vol 77 (5) ◽  
pp. 1288-1292 ◽  
Author(s):  
Nancy J Miller-Ihli

Abstract A method was developed for the determination of lead in sugars and syrups. Samples are wet-ashed with a nitric acid–hydrogen peroxide procedure and analyzed by graphite furnace atomic absorption spectrometry. The method involves the use of magnesium nitrate as a matrix modifier, air ashing, platform atomization, and quantitation by peak area measurements with direct calibration against aqueous standards. The instrumental detection limit (based on 3.29σ) was 10 pg, or 0.5 μg/L for a 20 μL injection, corresponding to a method detection limit of 3.3 ng/g sugar. The characteristic mass was approximately 12 pg. This method was validated by analyzing sucrose and high-fructose corn syrup samples spiked with known quantities of lead. The average recovery was 101 ± 6%.


1992 ◽  
Vol 75 (2) ◽  
pp. 334-340 ◽  
Author(s):  
Denis B Page, ◽  
Henry B.S Conacher, ◽  
Dorcas Weber, ◽  
Gladys Lacroix,

Abstract Recent findings of benzene In several fruit-flavored mineral waters at low μg/kg levels, reportedly arising from added benzoate, have prompted a survey of various fruits, juices, and drinks for traces of benzene. Headspace sampling, capillary gas chromatography, and mass spectrometrlc detection enabled detection with confirmation (full-scan spectrum) of benzene as low as 0.03 μg/kg. With selected Ion monitoring, the method detection limit was 0.02 μg/kg, I.e., 3 times the analytical blank, in total, 97 samples were analyzed. Benzene was found at levels ranging from 0.018 to 3.83 μg/kg. Samples labeled to contain added benzoate or believed to contain natural benzoate, such as cranberries, were found to contain benzene at higher levels (n = 41, av. 0.66 μg/kg) than other samples (n = 32, av. 0.082 μg/kg). Average levels of benzene In fruits (as expressed juice), In juices with and without benzoate, In noncarbonated drinks with and without benzoate, and in soft drinks with and without benzoate were 0.042,0.672,0.056,0.395, 0.116,0.793, and 0.062 μg/kg, respectively


2001 ◽  
Vol 84 (2) ◽  
pp. 368-375 ◽  
Author(s):  
Mohammed Rizk ◽  
Fathalla Belal ◽  
Fawiza Ibrahim ◽  
Soad Ahmed ◽  
Zeinab A Sheribah

Abstract A derivative UV-spectrophotometric analytical procedure was developed for determination of three 4-quinolone antibacterials: norfloxacin (NFX), ciprofloxacin (CFX), and sparfloxacin (SFX). The method depends on the complexation of Cu(II) with the studied compounds in aqueous medium. A third order, measurement was applied for their quantification. A linear correlation was established between the amplitude of the peak and concentration for all the studied drugs in the range of 15–80, 35–120, and 200–700 ng/mL, with minimum detectability (S/N = 2) of 1.0, 1.3, and 5.1 ng/mL for NFX, CFX, and SFX, respectively. The method was successfully applied for accurate, sensitive, and selective determination of the studied drugs in bulk and tablets formulation with average percentage recoveries of 99.22 ± 0.55 to 100.33 ± 1.60. The results obtained were favorably compared with those of the reference method. The method was also used to determine sparfloxacin in spiked human plasma and urine. The results obtained were satisfactory, accurate, and precise.


2014 ◽  
Vol 2014 ◽  
pp. 1-4
Author(s):  
T. Muhammad ◽  
A. Uzairu ◽  
M. S. Sallau ◽  
M. O. A. Oladipo

The Nigerian Research Reactor-1 was employed in the analysis of iodine in local food samples at an operating flux of 5.0×1011 ncm−2 s−1. Preconcentration neutron activation analysis (PCNAA) was compared against the most common spectroscopic (Sandell-Kolthoff reaction) technique, giving a concentration range of 0.295 to 2.960 mg/Kg and 0.264 to 2.725 mg/Kg, respectively, with an average percentage deviation of 11.34% and a positive correlation between the methods at 0.89. PCNAA and Sandell-Kolthoff spectroscopy of NIST 1548a reported values of 0.759±0.06 mg/Kg and 0.751±0.05 with Student’s t-test score of 1 and 0.95 and percentage standard deviation of 0 and 1.12%, respectively.


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