scholarly journals Validasi Metode Spektrofotometri Visible Untuk Penentuan Kadar Formaldehida Pada Pembalut Wanita Yang Beredar Di Pasaran

2017 ◽  
Vol 2 (1) ◽  
pp. 9-16
Author(s):  
Cicik Herlina Yulianti ◽  
Vika Ayu Devianti ◽  
M.A. Hanny Ferry Fernanda
Keyword(s):  
Limit Of Detection ◽  
Visible Spectrophotometry ◽  
Accuracy And Precision ◽  
Validation Criteria ◽  
Limit Of Quantitation ◽  
The Government ◽  
Nash Reagent ◽  
Positive Results ◽  
Specific Reagent

ABSTRAKPembalut menjadi kebutuhan wanita yang sangat penting karena digunakan untuk menyerap cairan darah ketika mengalami menstruasi. Pada pembuatan pembalut wanita dimungkinkan adanya pemakaian formaldehida. Oleh karena itu, pembalut wanita termasuk salah satu alat kesehatan yang kandungan dan bahan penyusunnya diatur oleh pemerintah. Pada penelitian ini menggunakan metode spektrofotometri visibel untuk penentuan kadar formaldehida dalam pembalut wanita sekali pakai. Sebelum digunakan, maka metode spektrofotometri visibel ini harus divalidasi terlebih dahulu untuk memastikan bahwa metode spektrofotometri yang digunakan dapat memberikan hasil yang akurat. Tujuan penelitian ini adalah melakukan validasi metode spektrofotometri visibel untuk penetapan kadar formaldehida dalam pembalut wanita sekali pakai menggunakan pereaksi nash sebagai reagen spesifik. Metode penelitian yang digunakan adalah pembuatan dan pembakuan larutan baku formaldehida, menentukan panjang gelombang maksimal, pembuatan kurva kalibrasi, melakukan uji linieritas, uji LOD dan LOQ, serta uji kesesuaian dan kecermatan, dan menentukan kadar formaldehida pada pembalut wanita. Hasil dari penelitian ini adalah bahwa metode spektrofotometri visibel memiliki selektifitas, linieritas,batas deteksi dan kuantitasi, presisi dan akurasi yang baik. Kadar rata-rata formaldehida pada ke lima sampel pembalut sebesar 2,88 mg/kg - 4,05 mg/kg.Kata kunci: pembalut, formaldehida, validasi, spektrofotometri visibelABSTRACTSanitary napkins are a very important woman’s need to absorb blood fluids when menstruating. In the manufacture of sanitary napkins may contain formaldehyde additives. Therefore, sanitary napkins are one of the medical devices whose composition is regulated by the government. In this study to identify the use of formaldehyde in sanitary napkins was carried out by visible spectrophotometry using nash reagent. This method should be validated in advance to ensure that the method used can provide accurate data. The aim of this research is to validate visible spectrophotometry method for determination of formaldehyde content indisposable sanitary napkins using nash reagent as specific reagent. Validation of UV – Vis spectrophotometry method for determination of formaldehyde showed that Nash reagent was suitable to determine formaldehyde. This method is linear with correlation coefficient (r2) of 0,99967. The validation characteristics include accuracy and precision, linearity, limit of detection, and limit of quantitation. The acceptance validation criteria were found in all case. Qualitative determination in five sanitary napkins samples showed positive results and the quantitative analysis confirmed that the average content of formaldehyde in five sanitary napkins samples was 2,88 mg/kg – 4,05 mg/kg.Keywords: sanitary napkins, formaldehyde, validation, visible spectrophotometry

scholarly journals Spectrophotometric Determination of Olmutinib in Bulk by Area under Curve and First Order Derivative Methods and its Validation as per ICH guidelines

2019 ◽  
Vol 9 (4-A) ◽  
pp. 349-354
Author(s):  
BALU KHANDARE ◽  
Atish C. Musle ◽  
Sanket S. Arole ◽  
Pravin V. Popalghat
Keyword(s):  
Area Under Curve ◽  
Limit Of Detection ◽  
Order Derivative ◽  
Spectrometric Method ◽  
First Order ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract: A simple, precise and economical UV-spectrophotometric method has been developed for the estimation of Olmutinib from bulk. Two methods were developed First method (A) applied was area under curve (AUC) in which the area was integrated in wavelength from 262-272nm. Second method (B) was first order derivative spectrometric method. In this method absorbance at λmin=256.57nm, λmax=282.83nm and zero cross=267.68nm was measured. Calibration curves were plotted for the method by using instrumental response at selected wavelength and concentration of analyte in the solution. In both the methods, linearity was observed in the concentration range of 2-12µg/ml at the λmax=267.68nm. Accuracy and precision studies were carried out and results were satisfactorily obtained. The drug at each of the 80 %, 100 % and 120 % levels showed good recoveries that is in the range of 98.00 to 99.00% for both methods, hence it could be said that the method was accurate. Limit of detection (LOD) and limit of quantitation (LOQ) were determined for the method. The method was validated as per International Conference on Harmonization. All validation parameters were within the acceptable limit. The developed method was successfully applied to estimate the amount of Olmutinib in pharmaceutical formulation.

scholarly journals Determination of Total Xanthone Content in the Preparation of Mangosteen Pericarp Capsules (garcinia mangostana l.) Available on the Market using UV-Visible Spectrophotometry Method

2019 ◽  
Vol 24 (2) ◽  
pp. 98 ◽  
Author(s):  
Delladari Mayefis ◽  
Yandri Anugerah ◽  
Roslinda Rasyid
Keyword(s):  
Limit Of Detection ◽  
Garcinia Mangostana ◽  
Visible Spectrophotometry ◽  
A Value ◽  
Limit Of Quantitation ◽  
Uv Visible ◽  
Market Needs ◽  
Interday Precision ◽  
Maximum Absorption Wavelength

The skin of Mangosteen fruit (Garcinia mangostana L.) is widely used as traditional medicine, for it contains a lot of xanthone compounds. Today, there are many products from mangosteen pericarp extract being sold on the market, one of which is the preparation of mangosteen pericarp capsules. Determining the total xanthone content in the preparation of mangosteen pericarp capsules (Garcinia mangostana L.) circulating on the market needs to be done to calculate the levels of xanthone that are not included in the preparation label. The results of the analysis with UV-Visible Spectrophotometry obtains the maximum absorption wavelength at 243 nm and the linear regression equation of the calibration curve that is y=0,0568+0,0727x with a value of r=0,9999. Validation of the analysis method showed the results of intraday precision obtained % RSD 0,34%, 0,17%, and 0,16%, interday precision of 0,23%, 0,35%, and 0,16%. The accuracy obtained was mean % recovery 95,55%, limit of detection 0,35 μg/ml and limit of quantitation 1,15 μg/ml. The results of the determination of the total xanthone content in the mangosteen pericarp capsules were 100,8 μg/mg in sample A; 197 μg/mg in sample B; and 50,2 μg/mg in sample C.

scholarly journals A Sensitive UV Spectrophotometric Method for the Determination of Gabapentin

2009 ◽  
Vol 6 (s1) ◽  
pp. S163-S170 ◽  
Author(s):  
R. Singh Gujral ◽  
S. Manirul Haque ◽  
P. Shanker
Keyword(s):  
Spectrophotometric Method ◽  
Good Accuracy ◽  
Limit Of Detection ◽  
Low Cost ◽  
Pharmaceutical Formulations ◽  
Accuracy And Precision ◽  
Ich Guidelines ◽  
Limit Of Quantitation ◽  
Precision Limit

An accurate and validated spectrophotometric method was developed for the determination of gabapentin. This is simple, sensitive and low cost UV spectrophotometric method. The method is based on the direct measurement of the native absorbance of the drug. The detection was done at 210 nm. The method was linear in the range of 0.25 - 3.5 µ g/mL with correlation coefficient of 0.9999. It is validated according to the ICH guidelines with respect to linearity, selectivity, accuracy and precision, limit of quantitation and limit of detection. The method has been applied to assess gabapentin in pharmaceutical formulations with good accuracy and precision and relatively free of interference from coexisting substances.

scholarly journals DETERMINATION OF Fe (II) IN KATUK LEAF (Saoropusandrogynus) CAPSULES USING UV-Vis SPECTROPHOTOMETER METHOD

2019 ◽  
Vol 9 (1) ◽  
pp. 44
Author(s):  
Tisa Mandala Sari
Keyword(s):  
Iron Content ◽  
Limit Of Detection ◽  
Analysis Method ◽  
Validation Criteria ◽  
Limit Of Quantitation ◽  
Uv Visible ◽  
R Value ◽  
Ion Analysis

Katuk leaf capsules generally use as ASI emitters and katuk leaf capsules also contain iron (II) which to prevent aneemia. Reseaerch on the determination of iron content in katuk leaf capsulse with UV-Visible spectrophotometricmethod has been done. The principle of this research is leuched dry katuk leaf capsulse with HCl 6 M. Then performed the determination rate of iron at 510 nm wavelength by way of reacting iron (II) with 1,10-phenantrolin. So that the complex is formed ferroin orange red. Validation of iron (II) ion analysis method in katuk leaf capsulse has fulfilled the validation criteria that is liniearity with r value = 0,9986, limit of detection (LOD) 0,3588µg/mL, limit of quantitation (LOQ) 1,1960µg/mL, iron (II) content in the sample SI 0,0153µg/mL, SII 0,0225µg/mL, and SIII 0,0268µg/mL. 

scholarly journals Development and Validation of a Rapid RP-HPLC Method for the Estimation of Esmolol Hydrochloride in Bulk and Pharmaceutical Dosage Forms

2010 ◽  
Vol 7 (3) ◽  
pp. 807-812 ◽  
Author(s):  
Vanita Somasekhar ◽  
D. Gowri Sankar
Keyword(s):  
Limit Of Detection ◽  
Hplc Method ◽  
Detector Response ◽  
Reverse Phase Hplc ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Development And Validation

A reverse phase HPLC method is described for the determination of esmolol hydrochloride in bulk and injections. Chromatography was carried on a C18column using a mixture of acetonitrile, 0.05 M sodium acetate buffer and glacial acetic acid (35:65:3 v/v/v) as the mobile phase at a flow rate of 1 mL/min with detection at 275 nm. The retention time of the drug was 4.76 min. The detector response was linear in the concentration of 1-50 μg/mL. The limit of detection and limit of quantification was 0.614 and 1.86 μg/mL respectively. The method was validated by determining its sensitivity, linearity, accuracy and precision. The proposed method is simple, economical, fast, accurate and precise and hence can be applied for routine quality control of esmolol hydrochloride in bulk and injections.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals STABILITY INDICATING HPLC METHOD FOR DETERMINATION OF VILAZODONE HYDROCHLORIDE

2017 ◽  
Vol 9 (4) ◽  
pp. 123
Author(s):  
Birva A. Athavia ◽  
Zarna R. Dedania ◽  
Ronak R. Dedania ◽  
S. M. Vijayendra Swamy ◽  
Chetana B. Prajapati
Keyword(s):  
Limit Of Detection ◽  
Degradation Products ◽  
Hplc Method ◽  
Alkaline Condition ◽  
Forced Degradation ◽  
Molecular Formula ◽  
Stability Indicating ◽  
Dry Heat ◽  
Limit Of Quantitation

Objective: The aim and objective of this study was to develop and validate Stability Indicating HPLC method for determination of Vilazodone Hydrochloride.Methods: The method was carried out on a Phenomenex, C18 (250x4.6 mm, 5 µm) Column using a mixture of Acetonitrile: Water (50:50v/v), pH adjusted to 3.3 with Glacial Acetic Acid for separation. The flow rate was adjusted at 1 ml/min and Detection was carried out at 240 nm.Results: The retention time of vilazodone hydrochloride was found to be 2.3 min. The calibration curve was found to be linear in the range 25-75µg/ml with a correlation coefficient (R2=0.996). The limit of detection and limit of quantitation were found to be 4.78µg/ml and 14.48µg/ml respectively. The % recovery of vilazodone hydrochloride was found to be in the range of 98.21±0.08 % to 99.07±0.64%. The proposed method was successfully applied for the estimation of vilazodone hydrochloride in marketed tablet formulation.Vilazodone Hydrochloride was subjected to forced degradation under Acidic, Alkaline, Oxidation, Dry Heat and Photolytic degradation conditions. Vilazodone hydrochloride showed 3.12% degradation under acidic condition, 4.78% under alkaline condition, 7.8% under oxidation condition, 3.53% under dry heat condition and 4.9% under photolytic condition.Acid degradation impurity was identified and characterised by LC-MS/MS was found to be 1-(4-Penten-1-yl) piperazine having molecular weight 154.253 (m/z 155.08) and Molecular Formula C9H18N2.Conclusion: A simple, precise, rapid and accurate Stability Indicating HPLC method has been developed and validated for the determination of Vilazodone Hydrochloride in presence of its degradation products as per the ICH Guidelines. 

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Determination of Simvastatin by Voltammetry Method at Screen-Printed Electrode Modified by Graphene Oxide Nanosheets and Sodium Dodecyl Sulfate

2022 ◽  
Author(s):  
Abolfazl Darroudi ◽  
Saeid Nazari ◽  
Seyed Ali Marashi ◽  
Mahdi Karimi-Nazarabad
Keyword(s):  
Graphene Oxide ◽  
Sodium Dodecyl Sulfate ◽  
Limit Of Detection ◽  
Sodium Dodecyl ◽  
Screen Printed Electrode ◽  
Support Electrolyte ◽  
Limit Of Quantitation ◽  
Dodecyl Sulfate ◽  
Screen Printed

Abstract An accurate, rapid, simple, and novel technique was developed to determine simvastatin (SMV). In this research, a screen-printed electrode (SPE) was deposited with graphene oxide (GO) and sodium dodecyl sulfate (SDS), respectively. For the first time, the handmade modified SPE measured the SMV by differential pulse voltammetry (DPV) with high sensitivity and selectivity. The results of cyclic voltammetry indicated the oxidation irreversible process of SMV. Various parameters (pH, concentration, scan rate, support electrolyte) were performed to optimize the conditions for the determination of SMV. Under the optimum experiment condition of 0.1 M KNO3 as support electrolyte and pH 7.0, the linear range was achieved for SMV concentration from 1.8 to 36.6 µM with a limit of detection (LOD), and a limit of quantitation (LOQ) of 0.06 and 1.8 µM, respectively. The proposed method was successfully utilized to determine SMV in tablets and urine samples with a satisfactory recovery in the range of 96.2 to 103.3%.

P–006 Simultaneous determination of bisphenol A and S in the samples of human seminal fluid

2021 ◽  
Vol 36 (Supplement_1) ◽  
Author(s):  
S Fialková ◽  
T Král ◽  
J Kohoutek ◽  
K Franzová ◽  
M Ješeta ◽  
...  
Keyword(s):  
Sample Preparation ◽  
Bisphenol A ◽  
Endocrine Disruptors ◽  
Analytical Method ◽  
Seminal Fluid ◽  
Limit Of Detection ◽  
Semen Parameters ◽  
Ms Detection ◽  
Validation Criteria ◽  
Limit Of Quantitation

Abstract Study question Can we quantitatively determine concentrations of endocrine disruptors namely bisphenol A and S in seminal fluid? Summary answer We developed selective analytical method to simultaneously screen for the presence of bisphenol A (BPA) and S (BPS). What is known already The male reproductive system involves processes, which may be influenced by the disruption of the endocrine system by chemicals called endocrine disruptors (EDs). There is a growing evidence that EDs such as bisphenol A and S may be responsible for the decline in male reproductive health. To date, the claimed adverse effects on male fertility are largely based on the results from studies assessing the relationship between urinary BPA and BPS concentration and semen parameters. The best evidence of an adverse effect of BPA and BPS directly on spermatozoa could be provided by measuring bisphenols concentration directly in seminal fluid. Study design, size, duration To selectively and quantitatively analyzed bisphenols in any biological matrix advanced analytical tools and selective sample preparation protocols must be employed. In this study we developed targeted analytical method based on liquid chromatography tandem mass (LC-MS/MS) detection to measure bisphenol A and S in seminal fluid samples obtained from IVF clinic. A total of 140 samples were analysed. Participants/materials, setting, methods BPA and BPS was extracted from 140 seminal fluid samples using solvent extraction followed by preconcentration step. Samples were analyzed on Agilent 6495 Triple Quadrupole (Agilent Technologies, Santa Clara, CA) operating in the ESI-negative mode. Two MS/MS transitions were used for quantitative LC-MS/MS analyses. Chromatographic separation was achieved on Waters™ ACQUITY™ UPLC™BEH C18 (100 × 2.1 mm, 1.7 µm) column using gradient elution with a mixture of 0.1mM ammonium fluoride and methanol as mobile phases. Main results and the role of chance We developed selective sample preparation method for detection of BPA and BPS in seminal fluid followed by LC-MS/MS detection. The method validation was performed based on FDA guidelines. Validation criteria included limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. Due to the lack of the certified reference material the validation criteria of the method were assessed in pool of spiked seminal samples. The accuracy of the LC-MS/MS method was evaluated as a percent recovery of the amount of target analyte added into the sample. Recovery rates were above 80% for both analytes. LOD was 0.04 ng/mL for BPA and 0.01 ng/mL for BPS. LOQ was 0.14 ng/mL and 0.02 ng/mL for BPS. Measured BPA concentration ranged from 0.04 ng/mL to 1.62 ng/mL. For BPS, the concentration ranged from 0.01 ng/mL to 0.47 ng/mL. BPA and BPS were detected in 64% and 81% of samples, respectively. Interestingly, BPA showed lower detection frequency compared to BPS. These results are consistent with other studies performed on urine samples. Limitations, reasons for caution The limitation of the developed method is the time-consuming sample preparation and analysis cost. Wider implications of the findings: These results document for the first time the presence of BPS in seminal fluid. Knowing the concentration of BPA and BPS in seminal fluid is crucial for mitigating the associated health risks and initiating intervention and prevention strategies. Our future work will evaluate the influence of BPS concentration on spermatozoa. Trial registration number AZV NV18–01–00544; CZ.02.2.69/0.0/0.0/19_074/0012727

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