Penetapan Kadar Metilparaben dalam Sediaan Krim Wajah yang Beredar di Kabupaten Pekalongan dengan Metode High Performance Liquid Chromatography (HPLC)

2021 ◽  
Vol 1 ◽  
pp. 1079-1087
Author(s):  
Mujtahida Rokhaitun Nikmah ◽  
Khusna Santika Rahmasari ◽  
W Wirasti ◽  
S Slamet

AbstractMethylparaben is a preservative that is often added in cosmetic preparations. The addition of methylparaben in cosmetics aims to protect the preparation from fungus so that cosmetic preparations are not easily damaged. The side effects of using methylparaben in the long term are irritation, allergic reactions, inflammation, and skin dermatitis. The purpose of this research was to analyze the content of methylparaben and determine the concentrationof metil paraben in the face cream samples. The qualitative test used Thin Layer Chromatography (TLC) method, mobile phases used were chloroform and methanol (9:1). Quantitative test used High Performance Liquid Chromatography (HPLC) method with methanol and aquabides as mobile phases (6:4). The results obtained in TLC are the sample Rf value is not much different from the standard Rf value, the standard Rf value is 0.60. Of the 10 samples analyzed, 8 spots appeared on samples 1, 2, 3, 4, 5, 6, 8, and 10 with an Rf value of 0.58, respectively; 0.57; 0.58; 0.57; 0.57; 0.57; 0.58; and 0.60. In the HPLC analysis, it was obtained that the sample levels in samples 1, 2, 3, 4, 5, 6, 8, and 10 were 0.33%, respectively; 0.30%; 1.21%; 0.29%; 0.52%; 0.44%; 0.41% and 1.14%. Samples 3 and 10 are not safe to use.Keywords: determination; face cream; preservative; methylparaben; HPLC. AbstrakMetilparaben adalah zat pengawet yang sering ditambahkan dalam sediaan kosmetik. Penambahan metilparaben dalam kosmetik bertujuan untuk menjaga sediaan agar terhindar dari jamur sehingga sediaan kosmetik tidak cepat rusak. Efek samping penggunaan metilparaben dalam jangka panjang yaitu dapat menimbulkan iritasi, reaksi alergi, inflamasi, dan dermatitis kulit. Tujuan dari penelitian ini adalah untuk menganalisis kandungan metilparaben dan mengetahui kadar metil paraben dalam sampel krim wajah. Pengujian secara kualitatif menggunakan metode Kromatografi Lapis Tipis (KLT), fase gerak yang digunakan yaitu kloroform dan metanol (9:1). Pengujian secara kuantitatif menggunakan metode High Performance Liquid Chromatography (HPLC) dengan fase gerak metanol dan aquabides (6:4).Hasil yang diperoleh pada KLT yaitu nilai Rf sampel tidak jauh berbeda dengan nilai Rf standar, nilai Rf standar sebesar 0,60. Dari 10 sampel yang dianalisis yaitu muncul 8 bercak pada sampel 1, 2, 3, 4, 5, 6, 8, dan 10 dengan nilai Rf berturut-turut yaitu sebesar 0,58; 0,57; 0,58; 0,57; 0,57; 0,57; 0,58; dan 0,60. Pada analisis HPLC diperoleh kadar sampel yaitu pada sampel 1, 2, 3, 4, 5, 6, 8, dan 10 secara berturut-turut sebesar 0,33%; 0,30%; 1,21%; 0,29%; 0,52%; 0,44%; 0,41% dan 1,14%. Sampel 3 dan 10 tidak aman untuk digunakan.Kata kunci: penetapan; krim wajah; pengawet; metilparaben; HPLC.

2021 ◽  
pp. 1-11
Author(s):  
Sultan M. Alshahrani ◽  
John Mark Christensen

This study was designed to develop and validate a simple and efficient high performance liquid chromatography (HPLC) method to determine flunixin concentrations in Asian elephant’s (Elephas maximus) plasma. Flunixin was administered orally at a dose of 0.8 mg/kg, and blood samples were collected. Flunixin extraction was performed by adding an equal amount of acetonitrile to plasma and centrifuging at 4500 rpm for 25 minutes. The supernatant was removed, and flunixin was analyzed using HPLC-UV detection. Two methods were developed and tested utilizing two different mobile phases either with or without adding methanol (ACN: H2O vs. ACN: H2O: MeOH). Both methods showed excellent linearity and reproducibility. The limit of detection was 0.05 ug/ml and limit of quantification was 0.1 ug/ml. the efficiency of flunixin recovery was maximized by the addition of methanol to mobile phase (ACN: H2O: MeOH as 50:30:20) at 95% in comparison to 23% without methanol. In conclusion, adding methanol to HPLC methods for extraction of flunixin from elephants’ plasma yielded higher recovery rate than without methanol.


2018 ◽  
Vol 2018 ◽  
pp. 1-11 ◽  
Author(s):  
Vinit V. Gholap ◽  
Leon Kosmider ◽  
Matthew S. Halquist

The use of electronic cigarettes (e-cigarettes) is a growing trend in population. E-cigarettes are evolving at a rapid rate with variety of battery powered devices and combustible nicotine refills such as e-liquids. In contrast to conventional cigarettes which are studied well for their toxicity and health effects, long-term clinical data on e-cigarettes are not available yet. Therefore, safety of e-cigarettes is still a major concern. Although the Food and Drug Administration (FDA) has recently started regulating e-cigarette products, no limits on nicotine and other ingredients in such products have been proposed. Considering the regulatory requirements, it is critical that reliable and standardized analytical methods for analyzing nicotine and other ingredients in e-cigarette products such as e-liquids are available. Here, we are reporting a fully validated high-performance liquid chromatography (HPLC) method based on nicotine peak purity for accurately quantifying nicotine in various e-liquids. The method has been validated as per ICH Q2(R1) and USP <1225> guidelines. The method is specific, precise, accurate, and linear to analyze nicotine in e-liquids with 1 to >50 mg/mL of nicotine. Additionally, the method has been proven robust and flexible for parameters such as change in flow rate, column oven temperature, and organic phase composition, which proves applicability of the method over wide variety of e-liquids in market.


2020 ◽  
Vol 20 (13) ◽  
pp. 1053-1059
Author(s):  
Mahmoud M. Sebaiy ◽  
Noha I. Ziedan

Background: Allergic diseases are considered as the major burden on public health with increased prevalence globally. Histamine H1-receptor antagonists are the foremost commonly used drugs in the treatment of allergic disorders. The target drug in this study, loratadine, belongs to this class of drugs and its biometabolite desloratadine which is also a non-sedating H1 receptor antagonist with anti-histaminic activity being 2.5 to 4 times greater than loratadine. This study aimed to develop and validate a novel isocratic Reversed-phase High-Performance Liquid Chromatography (RP-HPLC) method for rapid and simultaneous separation and determination of loratadine and its metabolite, desloratadine in human plasma. Methods: The drug extraction method from plasma was based on protein precipitation technique. The separation was carried out on a Thermo Scientific BDS Hypersil C18 column (5μm, 250 x 4.60 mm) in a mobile phase of MeOH: 0.025M KH2PO4 adjusted to pH 3.50 using orthophosphoric acid (85: 15, v/v) at an ambient temperature. The flow rate was maintained at 1 mL/min and maximum absorption was measured using the PDA detector at 248 nm. Results: The retention times of loratadine and desloratadine in plasma samples were recorded to be 4.10 and 5.08 minutes, respectively, indicating a short analysis time. Limits of detection were found to be 1.80 and 1.97 ng/mL for loratadine and desloratadine, respectively, showing a high degree of sensitivity of the method. The method was then validated according to FDA guidelines for the determination of the two analytes in human plasma. Conclusion: The results obtained indicate that the proposed method is rapid, sensitive in the nanogram range, accurate, selective, robust and reproducible compared to other reported methods.


1986 ◽  
Vol 49 (5) ◽  
pp. 383-388 ◽  
Author(s):  
PETER SPORNS ◽  
SUET KWAN ◽  
LAWRENCE A. ROTH

Oxytetracycline (OTC), also known commercially as Terramycin, was determined to be more stable in honey than in buffered aqueous solutions at similar pH values and temperatures. A rapid high performance liquid chromatography (HPLC) method was developed to detect and quantitate OTC using a 1:1 dilution (wt/wt) of honey samples in water. Using 355 nm as the wavelength of detection, amounts as low as 0.5 μg/ml could be detected in the above solution. The limits of detection were lowered considerably by a double extraction procedure.


2006 ◽  
Vol 89 (6) ◽  
pp. 1552-1556
Author(s):  
ArmaĞan Önal ◽  
Olcay SaĞiri ◽  
S Müge Çetin ◽  
Sidika Toker

Abstract Reboxetine is used as a selective noradrenaline reuptake inhibitor for the treatment of major depressive disorders. It is effective in the treatment of severe depression and safer to use than traditional tricyclic antidepressants. In this study, a novel, simple, and rapid stability-indicating high-performance liquid chromatography (HPLC) method for reboxetine methansulfonate was successfully developed and validated for the assay of tablets. The method was used to quantify reboxetine in tablets; it employed a C18 column (150 4.6 mm id) with an isocratic mobile phase consisting of methanolphosphate buffer (pH 7, 0.02 M; 55 + 45, v/v) at a flow rate of 1.0 μmL/min. Reboxetine was detected by an ultraviolet detector at 277 nm. The retention time of reboxetine was about 4.5 min. The developed HPLC method was validated with respect to linearity, precision, sensitivity, accuracy, and selectivity. The method was linear over the concentration range 150 g/mL (r 0.9999). The limits of detection and the quantitation of reboxetine were 0.1 and 0.3 μg/mL, respectively. The relative standard deviation values for intraday and interday precision were 0.781.01 and 1.081.37%, respectively. Selectivity was validated by subjecting a stock solution of reboxetine to neutral, acid, and alkali hydrolysis, as well as oxidation, dry heat treatment, and photodegradation. The peaks of the degradation products did not interfere with the peak of reboxetine. The results indicated that the proposed method could be used in a stability assay. The proposed method was successfully applied to the determination of reboxetine in tablets. Excipients present in the tablets did not interfere with the analysis.


2021 ◽  
Vol 0 (0) ◽  
Author(s):  
Katso Binang ◽  
David T. Takuwa

Abstract The aim of the study was to develop a rapid, efficient, and cheap chromatographic method for determining four selected antihypertensive active flavonoid compounds in medicinal plants in Botswana. The determination of rutin, quercetin, and kaempferol in selected medicinal plants was conducted in less than 6 min using the developed reverse phase-high performance liquid chromatography (RP-HPLC) method with a 2.7 µm Ascentis C18 express column (150 × 4.60 mm i.d) at 340, 360, and 368 nm detection wavelengths and mobile phase of methanol and 0.068% of formic acid solution in isocratic elution. Validation results showed good selectivity, linearity (r 2 > 0.99), high percentage recoveries (90.2–104.7%), and precision (% RSD < 2) for n = 3, confirming suitability of the method for determination of the investigated flavonoids in Zingiber officinale (ginger). Application of the developed RP-HPLC method was performed in selected medicinal plants (Lippia javanica ) (mosukujane), Myrothanmus flabellious (galalatshwene), and Elephantorrhiza elephantina (mositsana) used to manage hypertension by herbalists in Botswana. M. flabellious a very commonly used plant for managing hypertension was found to contain highest amounts of rutin and myricetin, whereas nothing was detected for E. elephantina.


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