scholarly journals Validasi Metode Analisis Formaldehid Pada Tisu Basah

2018 ◽  
Vol 3 (2) ◽  
pp. 47-50
Author(s):  
Dwi Wahyuniati ◽  
Cicik Herlina Yulianti ◽  
Mercyska Suryandari
Keyword(s):  
Method Validation ◽  
Limit Of Detection ◽  
Liquid Composition ◽  
Regenerated Cellulose ◽  
General Terms ◽  
Percent Recovery ◽  
Limit Of Quantitation ◽  
Wet Condition ◽  
Recovery Study ◽  
Nash Reagent

ABSTRAKTisu basah merupakan istilah umum untuk menggambarkan sepotong bahan, umumnya ditambahkan dengan komposisi cairan atau semi cair, dimaksudkan untuk membersihkan dan memberikan rasa lembut. Tisu basah memiliki struktur berserat terdiri dari campuran serat selulosa pulp dan regenerasi, seperti rayon dan atau liosel, dengan atau tanpa serat pengikat. Pada proses produksi, komponen-komponen yang sengaja ditambahkan pada pembuatan tisu basah salah satunya adalah formaldehid sebagai penguat keadaan basah. Akan tetapi penggunaan yang berlebihan dapat menyebabkan ruam pada kulit (dermatitis). Pada penelitian ini dilakukan validasi metode analisis formaldehid pada tisu basah dengan menggunakan metode absorpsi uap SNI ISO 14184-2:2015 dengan pereaksi nash menggunakan spektrofotometri UV-Vis. Sampel yang digunakan adalah tisu basah dari satu merek. Validasi metode dilakukan untuk memastikan metode SNI ISO 14184-2:2015 dapat diterapkan, diperoleh hasil valid, dengan nilai R = 0,9993, yang mendekati nilai 1, menghasilkan persamaan regresi linier y = 0,0294x - 0,0317. Pengujian akurasi diperoleh rata-rata persen recovery sebesar 84,54%, 102,05%, dan 106,13%. Nilai RSD sebesar 1,62%. Hasil nilai LOD sebesar 0,040, sedangkan hasil nilai LOQ sebesar 0,136. Hasil validasi terhadap metode SNI ISO 14184 – 2 : 2015 dapat disimpulkan bahwa metode SNI ISO 14184-2:2015 dapat digunakan untuk menguji formaldehid pada tisu basah. Kata kunci: Validasi, Tisu basah, Formaldehid, Pereaksi Nash, Spektrofotometri UV-Vis.ABSTRACT Wet wipes are the general terms to describe a piece of material, generally impregnated with a liquid or semi liquid composition, intended to both cleaning and providing a smooth feeling. Wet wipes has fibrous structures consist of a mixture of pulp and regenerated cellulose fibers, such as rayon and/or lyocell, with or without binding fibers. In product process, one of components expressly added was formaldehyde as strengthener as wet condition. But, excessive use of formaldehyde can cause skin rash (dermatitis). This study was aimed to Analysis Method Validation of Formaldehyde of Wet Wipes used vapour absorption SNI ISO 14184-2:2015 method with Nash Reagents by UV-Vis Spectrophotometry, and used vapour absorption method. The wet wipes sample used was from one brand. Method validation was conducted to definite SNI ISO 14184-2:2015 method can be applied, the result was valid, r value is 0,9993, the linear regression y = 0,0294x – 0,0317, accuracy percent recovery study showed 84,54%, 102,05%, and 106,13%., Related standar deviation showed 1,62%, limit of detection was 0,040, limit of quantitation was 0,136. The validation result of SNI ISO 14184-2:2015 method can be concluded that SNI ISO 14184-2:2015 method can be applied to examine formaldehid on wet wipes.Keywords: Wet wipes, Formaldehyde, Validation, Nash Reagent, UV-Vis Spectrophotometry.

scholarly journals THE RAPID AND GREEN HAIR ANALYSIS METHOD DEVELOPMENT USING FTIR FOR PAPAVERINE HCL DETERMINATION

2019 ◽  
pp. 211-217 ◽  
Author(s):  
ILMA NUGRAHANI ◽  
STEPHANIE SULISTIANA ◽  
SLAMET IBRAHIM
Keyword(s):  
Hair Sample ◽  
Method Development ◽  
Limit Of Detection ◽  
Area Under The Curve ◽  
Forensic Analysis ◽  
Percent Recovery ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Papaverine Hydrochloride

Objective: This study was aimed to develop a rapid analysis using FTIR (Fourier Transform Infra-Red) for papaverine hydrochloride (HCl) determination in the hair sample, supported by a mathematically manipulation; which never been reported before in toxicology and forensic analysis. Methods: Firstly, the method was checked its validity to ensure the feasibility for the quantitative purpose. The absorbance spectrums were collected by measure the drug, matrix, and its mixture. A spectra which showed the best specificity and linearity then was selected and derived. Afterwards, the area under the curve (AUC) was measured. A series of concentration was used for compose the calibration curve. Based on the result, some validation parameters were checked thoroughly. Further, for sample preparation, hair was collected non-invasively, then was decontaminated using soap. Next, it was immersed into a papaverine HCl solution at a concentration of 25 mg/ml along days. Finally, the amount of drugs absorbed were measured by the developed method using FTIR. Results: Experimental data showed that all validation parameters could be fulfilled by the developed method. The selected spectra for the content determination was 1320-1230 cm-1. Its linearity was represented by a correlation coefficient value (r) ≥ 0.9999, variation coefficient (Vxo) ≤ 2.0%. The limit of detection (LOD) was 0.00618% w/w, meanwhile, the limit of quantitation (LOQ) was 0.02060% w/w, respectively. The percent recovery was in the range 97-103% with the relative standard deviation (RSD) was ≤ 2.0%. The drug has detected after 72 h immersion, moreover, after 192 h the concentration gained was 0.1594±0.0011% w/w. Conclusion: As the conclusion, FTIR absorbance-derivative method is adequate as a rapid procedure for determine papaverine HCl in the hair sample. This method shows the appropriate of specificity, accuracy and precise. In addition, it shows the advantages of simplicity, green/eco-friendlier, and cost-efficiency.

scholarly journals METHOD VALIDATION FOR ORGANOCHLORINE INSECTICIDES DETERMINATION IN GINSENG BY USING ISOTOPE-DILUTION GAS CHROMATOGRAPHY-MASS SPECTROMETRY (ID-GC-MS)

2020 ◽  
Vol 17 (34) ◽  
pp. 362-372
Author(s):  
Yosi ARISTIAWAN ◽  
Dillani PUTRI RAMADHANINGTYAS ◽  
Isna KOMALASARI ◽  
Dyah STYARINI ◽  
Nuryatini HAMIM
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Method Validation ◽  
Isotope Dilution ◽  
Limit Of Detection ◽  
Plant Protection ◽  
Gas Chromatography Mass Spectrometry ◽  
Chromatography Mass Spectrometry ◽  
Organochlorine Insecticides ◽  
Limit Of Quantitation

Organochlorine insecticides are still exploited among the most prominent pesticides for plant protection purposes. Known for having hazardous to humans and persistent in the environment properties, it is necessary to build an accurate method for detecting organochlorine insecticides in food and environmental substances. Isotope-dilution gas chromatography-mass spectrometry (ID-GC-MS) is a versatile coupling measurement system and high order method that combines both selectivity, sensitivity and high accuracy. The present paper aims at showing the methodology of the organochlorine insecticides (alpha-HCH and gamma-HCH) determination in ginseng by using ID-GC-MS. The described method covered sample preparation using an organic solvent (hexane) extraction, followed by florisil cleaning-up. After the reconstitution of the solvent base, the measurement was conducted by using ID-GC-MS in the optimal instrument parameter. Using the determined optimal conditions, the parameters such as sensitivity, linearity, precision, and accuracy were studied for validation of the ID-GC–MS method. The limit of detection and the limit of quantitation of the instrument were 0.5 ng/g and 2.0 ng/g for both analytes. The method showed linearity with the correlation coefficient of 0.999 for both alpha-HCH and gamma-HCH over the concentration range of 1‒300 ng/g. The precision ranged from 3.0 to 3.7% and 2.4 to 3.3% for alpha-HCH and gamma-HCH, respectively. The mean recoveries for alpha-HCH and gamma-HCH were found at 98.0 and 95.6%, respectively. Following method validation, the measurement uncertainty of the alpha-HCH and gamma-HCH determination was evaluated according to EURACHEM GUM guide at a 95 % confidence level (k = 2). The expanded uncertainty in the measurement of alpha-HCH and gamma-HCH was 5.4% and 8.2%, respectively. All these parameters demonstrate the high sensitivity of the offered method and the success of the described method in the determination of alpha-HCH and gamma-HCH in ginseng sample.

scholarly journals Cost Effective, Efficient and Stability indicating Method Development & Validation for determination of related substances for Levonorgestrel & Ethinyl Estradiol Tablets

2021 ◽  
Vol 11 (2) ◽  
pp. 153-163
Author(s):  
Abhiram Dash ◽  
Neelu Jain ◽  
Harish Pandey
Keyword(s):  
Method Validation ◽  
High Performance ◽  
Method Development ◽  
Ethinyl Estradiol ◽  
Limit Of Detection ◽  
Cost Effective ◽  
Hplc Method ◽  
Related Substances ◽  
Limit Of Quantitation

The objective of this research was to develop and validate a simple, specific and accurate reverse phase of high performance of liquid chromatographic method for the determination of levonorgestrel (LVG) and ethinylestradiol (EE) in tablets. The chromatographic system included column Sun Fire ODS (150 mm × 4.6 mm i.d., particle size at 5 μm), mobile phase consisting of acetonitrile: methanol: aquabidest (60:15:25) with the flow rate of 1 mL/minute and effluents monitored at 230 nm. The validation of RP HPLC method for the simultaneous determination of LVG and EE was determined by accuracy, precision, linearity, and limit of detection (LOD) as well as the limit of quantitation (LOQ) parameters. The linearity range of both drugs was 1-70 µg/mL and 2-14 µg/mL for LVG and EE, respectively. The recoveries of LVG and EE were at 101.78% and 102.44% with the coefficients of variation of 0.94% and 1.92%, successively. The LOD of LVG and EE value were of 0.84 µg/mL and 0.03 µg/mL, and LOQ value were of 2.79 and 0.09µg/mL, respectively. Keywords: Levonorgestrel (LVG), Ethinylestradiol, Method Validation, Method Validation, HPLC

Validation of Methods Used in the Florida Department of Agriculture and Consumer Services' Chemical Residue Laboratory

1991 ◽  
Vol 74 (5) ◽  
pp. 868-871 ◽  
Author(s):  
Gail Abbott Parker
Keyword(s):  
Method Validation ◽  
Method Development ◽  
Limit Of Detection ◽  
Collaborative Study ◽  
Raw Milk ◽  
Development Project ◽  
Limit Of Quantitation ◽  
Chemical Residue ◽  
Consumer Services ◽  
Validation Scheme

Abstract Very few methods for detecting residues of pesticides in food or agricultural samples have undergone rigorous collaborative study and possess official AOAC status. The Chemical Residue Laboratory has formalized a method validation scheme to use when incorporating or developing new, unofficial methods. These methods are validated by assessing certain performance parameters: scope, specificity, linear range, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ). For accuracy and precision assessment, 12 replicate fortifications must yield recoveries within the range of 70-120% with a coefficient of variation (CV) that compares favorably to the Horwitz CV. LOD and LOQ are equivalent to 3 and 10 times, respectively, the background signal contributed by a sample matrix blank. This criterion that we use for LOD/LOQ is not universal. In fact, because of differing definitions, we have encountered difficulties in enforcing a tolerance by using a registrant's method. This paper also presents an example of our method validation scheme, using a recent method development project for detecting sulfamethazine in raw milk. The sulfamethazine project also revealed unanticipated personnel problems, underscoring the importance of the human factor in quality assurance.

scholarly journals Validation of High-Performance Liquid Chromatography Method for Determination of Vitamin B1 in Powder Milk

2020 ◽  
Vol 23 (5) ◽  
pp. 177-182
Author(s):  
Supriyono Supriyono ◽  
Mudhiah Fitrillah ◽  
Arie Pratama Putra
Keyword(s):  
Method Validation ◽  
Limit Of Detection ◽  
Milk Powder ◽  
Vitamin B1 ◽  
Enzymatic Reactions ◽  
System Suitability ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Vitamin B1 plays an important role in the co-enzymatic reactions for energy-rich compounds called ATP (Adenosine Tri Phosphate). Therefore, it should be added to various food products, for example, milk powder. One method that can be used to determine vitamin B1 is SNI number 3751: 2009, but the method is intended for wheat flour. If the method is to be used for the analysis from other samples, such as milk powder, optimization, and validation, are needed. This experiment was carried out using HPLC, C18 column, and UV detector with a wavelength of 254 nm. The mobile phase used is methanol: acetic acid: bi-distilled water = 32:1:67 (v/v/v), flow rate = 1 mL/minute, isocratic, and reverse phased technique. Method validation parameters include tests of system suitability, linearity, the limit of detection, the limit of quantitation, precision (repeatability), and accuracy. The results showed that the system suitability test was obtained relative standard deviations (% RSD) for retention time and peak area, tailing factor, resolution, separation factor was 0.297%, 1.476%, 1.113, 6.693, and 4.406 respectively. The validation test gets a correlation coefficient (R) of 0.9996, the limit of detection and limit of quantitation were 0.0122 mg/100 mL and 0.0244 mg/100 mL, respectively. The precision test obtained Horwitz's ratio of 0.27%. Accuracy test using CRM obtained % recovery of 93.79-97.77%. All these results meet the requirements of method validation, so it can be concluded that the method of SNI number 3751: 2009 is valid for the determination of vitamin B1 in milk powder and can be used for routine analysis procedure.

DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC METHOD FOR THE ESTIMATION OF ROTIGOTINE IN NANOSTRUCTURED LIPID CARRIERS

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (08) ◽  
pp. 61-67
Author(s):  
Jagruti B. Prajapati ◽  
Gayatri Patel ◽  
Keyword(s):  
Correlation Coefficient ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Nanostructured Lipid Carriers ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Recovery Study ◽  
Nanostructure Lipid Carriers ◽  
Development And Validation

Rotigotine (RTG) loaded Nanostructure Lipid Carriers (NLCs) were developed for the treatment of Parkinson’s disease. To estimate RTG entrapped in NLCs, UV spectrophotometric method was developed and validated. The solvent and wavelength of detection were optimized in order to maximize sensitivity of the proposed method. The method was validated for different parameters like linearity, precision, specificity, accuracy, limit of detection (LOD), limit of quantitation (LOQ) and robustness as per ICH guidelines. A wavelength maximum of RTG in methanol: chloroform (6:4V/V) mixture was found at 273 nm. The method was found to be linear in the range of 40 to 200 µg/mL with a correlation coefficient (r2 ) of 0.998. The accuracy of the method was studied by recovery study and % recovery was found in range of 99 to 100.37 %. The LOD and LOQ were found to be 0.09 µg/mL and 6.1 µg/mL, respectively. The method is simple, accurate and requires relatively inexpensive instrument. The method was used successfully for determination of RTG loaded into NLCs.

DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRIC METHOD FOR THE ESTIMATION OF AGOMELATINE IN NANOSTRUCTURED LIPID CARRIERS

INDIAN DRUGS ◽  
2017 ◽  
Vol 54 (03) ◽  
pp. 52-57
Author(s):  
S. D Verma ◽  
J. B. Prajapati ◽  
A. A. Patel ◽  
Keyword(s):  
Correlation Coefficient ◽  
Spectrophotometric Method ◽  
Limit Of Detection ◽  
Nanostructured Lipid Carriers ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Recovery Study ◽  
Development And Validation

The objective of work was to develop and validate a UV spectrophotometric method for determination of agomelatine (AGM) loaded in nanostructured lipid carriers (NLCs). The solvent and wavelength of detection were optimized in order to maximize sensitivity of proposed method. The method was validated for different parameters like linearity, precision, specificity, accuracy, limit of detection (LOD), limit of quantitation (LOQ) and robustness as per ICH guidelines. A wavelength maximum of AGM in methanol: chloroform (7:3V/V) mixture was found at 235nm. The method was found to be linear in the range of 1 to 6μg/mL with a correlation coefficient (r2) of 0.997. The accuracy of the method was studied by recovery study and % recovery was found in range of 99 to 100.11%. The LOD and LOQ were found to be 0.043μg/mL and 0.141μg/mL respectively. The method is simple, accurate and requires relatively inexpensive instrument. The method was used successfully for determination of AGM loaded into NLCs.

scholarly journals Assessment of toxic and essential heavy metals in imported dried fruits sold in the local markets of Jordan

2018 ◽  
Vol 9 (4) ◽  
pp. 394-399
Author(s):  
“Ayat Allah” Al-Massaedh ◽  
Ahmad Gharaibeh ◽  
Samah Radaydeh ◽  
Idrees Al-Momani
Keyword(s):  
Heavy Metals ◽  
Limit Of Detection ◽  
Average Concentration ◽  
Flame Atomic Absorption Spectroscopy ◽  
Flame Atomic Absorption ◽  
Percent Recovery ◽  
Limit Of Quantitation ◽  
Fruit Samples ◽  
Dried Fruit ◽  
Good Agreement

In the present study, the concentrations of nine heavy metals (Fe, Zn, Mn, Cu, Mg, Cr, Ni, Cd, and Pb) in six different imported dried fruit samples of different brands (Mangoes, black raisins, figs, apricots, plums, and cranberries) were determined by Flame Atomic Absorption Spectroscopy (FAAS) after wet digestion. Samples were collected from different stores in Amman, Jordan. The average concentration of the selected metals in the analyzed samples were found to be in the range of 1.70-8.70 (Fe), 0.15-0.72 (Zn), 0.09-0.59 (Mn), 0.07-0.46 (Cu), 2.5-53.4 (Mg), 0.06-0.15 (Cr), 0.17-0.29 (Ni), 0.01-0.05 (Cd), and 0.11-0.57 (Pb) µg/g. The highest concentrations of Fe, Zn, Mn, Mg, and Ni were found in dried figs, highest concentrations of Cr, Cd, and Pb were found in dried apricots, and highest concentrations of Cu was found in dried black raisins. The results obtained in this study showed that Mg and Fe have the highest concentrations in all analyzed samples, whereas, the lowest concentrations obtained were for Cd and Cr. The concentrations of the highly toxic metals (Pb and Cd) in the all analyzed samples were found to be below or in good agreement with the permissible limits set by different health organizations. The figures of merit obtained for the FAAS calibration curves are brilliant with good linearity (r2 > 0.99). The FAAS method was validated by determining limit of detection (LOD), limit of quantitation (LOQ), and percent recovery (%R) for all investigated metals. The results obtained in this work were compared with the literature reported values.

scholarly journals A simple Simultaneous UV Spectrophotometric Method to Determine Isoniazid and Rifampicin Contents in One Combined Tablet

2020 ◽  
Vol 11 (SPL4) ◽  
pp. 1982-1988
Author(s):  
Zilhadia Zilhadia ◽  
Supandi Supandi ◽  
Adha Dastu Ilahi
Keyword(s):  
Method Validation ◽  
Limit Of Detection ◽  
Simultaneous Analysis ◽  
Uv Spectrophotometry ◽  
Limit Of Quantification ◽  
Accuracy Test ◽  
Advanced Phase ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Limit Of Quantitation

Isoniazid and rifampicin are the first-line anti-tuberculosis drugs in the advanced phase. This study aimed at validating the method to determine the levels of isoniazid and rifampicin contents in one serve of combined tablet circulating at Pramuka market using simultaneous analysis of Ultraviolet Spectrophotometry with methanol as a solvent. The maximum wavelength of isoniazid and rifampicin obtained was 261 nm and 337 nm, respectively. The method used to confirm the validity here includes linearity, the limit of detection (LOD), limit of quantitation (LOQ), accuracy, and precision under the ICH guidelines. The results of the method validation for isoniazid and rifampicin were as follow: linearity (R2) in the range 5-25 µg / mL showed about 0.9998 and 0.9997, the limit of detection (LOD) 0.4026 µg/mL and 0.4952 µg / mL, and the limit of quantification (LOQ) 1.3421 µg / mL and 1.6508 µg / mL respectively. Besides, the accuracy-test (% recovery) was in the range of 100.44% ± 0.41% to 107.26% ± 0.28%, while the precision test (% RSD) was less than 2%. The determination of the contents was carried out on samples purchased at Pramuka Market with predetermined criteria and obtained levels of active ingredients ranging from 92.774% ± 0.39% to 103.51% ± 0.41%. The method validation to determine the levels of isoniazid and rifampicin contents in one serve of combined tablet using simultaneous analysis of Ultraviolet (UV) Spectrophotometry with methanol as a solvent is recommended for preparation analysis at the market.

scholarly journals Simultaneous HPTLC Estimation of Simvastatin and Ezetimibe in Tablet Dosage Form

2010 ◽  
Vol 7 (4) ◽  
pp. 1206-1211 ◽  
Author(s):  
Bhupendra Shrestha ◽  
B. Stephenrathinaraj ◽  
Sita Sharan Patel ◽  
N. K. Verma ◽  
R. Mazumder
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
High Performance ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Percent Recovery ◽  
Limit Of Quantitation ◽  
The Mean ◽  
Tablet Dosage ◽  
Layer Chromatography

A method enabling the precise and quick simultaneous analysis of simvastatin and ezetimibe in tablet formulation by high performance thin layer chromatography has been presented. Samples of simvastatin and ezetimibe in organic solvents were separated on a plate coated with silica gel 60 F-254 and the chromatograms were developed using a mixture of chloroform and methanol (9.5: 0.5 %v/v). The method has a linearity range of 40-280 ng.mL-1for both the drugs when scanned at 254 nm. The limit of detection and limit of quantitation was found to be 30 and 100 ng.band-1respectively, for both the drugs. The mean percent recovery was found to be 100.65 and 101.55 for simvastatin and ezetimibe. The intra-day and inter-day precision studies were carried out with mean RSD of 0.88 and 1.27 for ezetimibe and 1.35 and 1.50 for simvastatin.

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