Separation and Determination of Synthetic Impurities of Sildenafil (Viagra) by Reversed-Phase High-Performance Liquid Chromatography

Nagaraju, V.; Sreenath, Dasari; Rao, J. T.; Rao, R. Nageswara

doi:10.2116/analsci.19.1007

Cited by 24 publications

(12 citation statements)

References 13 publications

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“…Several techniques are reported for the determination of SDF in many kinds of food supplements and pharmaceutical formulations, namely flow injection analysis, 2 thin layer chromatography (TLC), 12 spectrophotometry, 2,13 spectrofluorometry, 14 high-performance liquid chromatography (HPLC)-ultraviolet (UV), 7,[15][16][17] HPLC-diode array detection, 12,18 HPLC-electrospray ionization-mass spectrometry (ESI-MS), 19 micellar electrokinetic chromatography, 4 electrospray tandem (ESI)-MS, 11 gas chromatography (GC)-MS, 20,21 liquid chromatography (LC)-MS, 12 and LC-MS. 22,23 In addition, low analytical sensitivity, inadequate intraday and interday reproducibility values, and inappropriate recovery amounts cause problems with the use of these techniques. 7,1 (%RE) arasındaydı.…”

Section: Introductionmentioning

confidence: 99%

Investigation of the Presence of Sildenafil in Herbal Dietary Supplements by Validated HPLC Method

Dural¹

2020

tjps

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Amaç: FDA tarafından onaylı ilk fosfodiesteraz-5 inhibitörü olan sildenafil (SDF), güçlü farmakodinamik etkinliği sebebiyle erektil fonksiyon bozukluğunun tedavisinde yaygın olarak kullanılmaktadır. Günümüzde birçok gıda takviyesi, yasadışı tağşiş işlemlerine dahil olduğundan, gıda takviyelerinin içerisindeki SDF varlığının belirlenmesi toksikolojik riskleri sebebiyle çok önemlidir. Bu çalışmada bitkisel gıda takviyelerinde (BGT) SDF analizi için basit, hızlı, güvenilir bir ultraviyole (UV) detektörlü yüksek performanslı sıvı kromatografi yöntemi geliştirilmiş ve valide edilmiştir. Gereç ve Yöntemler: Mobil faz olarak içeriğinde %0,1 trietilamin bulunan 10 mM'lik fosfat tamponu (pH 3,5) ve asetonitril (65:35, v/v) bir ters faz C18 analitik kolonuna (4,6×250 mm, 5 µm) izokratik olarak uygulanmıştır. Mobil faz akış hızı 1 mL dk-1 ve kolon sıcaklığı 35°C idi. UV dedektör 293 nm'ye ayarlanmıştır. Çalışmada kullanılan sıvı-sıvı ekstraksiyon yöntemi, BGT'lerde SDF'nin geri kazanımı için basit ve pratik bir yöntem sağladı ve elde edilen değerleri %87,6 ila 111,7 arasındaydı. Bulgular: Yöntem, mükemmel bir korelasyon katsayısı ile doğrusallık göstermiştir (r 2 >0,999). Ayrıca, metot 6,5 ng mL-1 'lik tayin limitiyle seçici ve hassastı. Gün içi ve günler arası metot kesinlik ≤%8,2 (% bağıl standart sapma) idi. Gün içi ve günler arası metot doğruluk testi sonuçları (-4,0) ile ABSTRACT Objectives: As the first FDA-approved phosphodiesterase type 5 inhibitor, sildenafil (SDF) is widely used in the treatment of erectile dysfunction due to its strong pharmacodynamic activity. Since many food supplements are now involved in illegal adulteration, the presence of SDF in food supplements is very important because of their toxicological risks. In this study a simple fast, reliable high-performance liquid chromatography method with ultraviolet (UV) detector has been developed and validated for SDF analysis in herbal dietary supplements (HDSs). Materials and Methods: 10 mM phosphate buffer containing 0.1% triethylamine (pH 3.5) and acetonitrile (65:35, v/v), as mobile phase was applied isocratically to a reverse phase C18 analytical (4.6×250 mm, 5 µm) column. Chromatographic separation was achieved by a C 18 reverse-phase analytical column 4.6×250 mm, 5 µm particle size, using acetonitrile, with 10 mM phosphate buffer containing 0.1% triethylamine (65:35, v/v, pH 3.5) as a mobile phase. The mobile phase flow rate was 1 mL min-1 and the column temperature was 35°C. The UV detector was set at 293 nm. The liquid-liquid extraction method used in the study provided a simple and practical method for the recovery of SDF in HDSs and their obtained values ranged from 87.6 to 111.7%. Results: The method showed linearity with an excellent correlation coefficient (r 2 >0.999). Moreover, it was specific and sensitive with the limit of quantification, 6.5 ng mL-1. Intraday and interday method precision was ≤8.2 (relative standard deviation %). Intraday and interday method accuracy was between-4.0 and 7.1 (RE%). The method was strong according to th...

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Section: Introductionmentioning

confidence: 99%

Investigation of the Presence of Sildenafil in Herbal Dietary Supplements by Validated HPLC Method

Dural¹

2020

tjps

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“…Various synthetic PDE-5 inhibitors combined with the complex herbal matrix make the detection difficult, even with the most sophisticated instrumentation. Several reported methods for the determination of sildenafil including widely used HPLC technology [10][11][12][13][14][15], capillary electrophoresis [16], LC-MS [17], together with sample pretreatment methods such as solid-phase extraction (SPE), liquid-liquid extraction (LLE), etc. Among these, SPE can be applied readily to a wide range of compounds because of its broad range of sorbents available on the market.…”

Section: Introductionmentioning

confidence: 99%

Synthesis of core–shell magnetic molecularly imprinted polymers and detection of sildenafil and vardenafil in herbal dietary supplements

Ding

Yuan

et al. 2011

Journal of Hazardous Materials

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“…Spectrophotometric method based either on the formation of yellow chromogen with sodium nitropruside and hydroxylamine or formation of violet colored chromogen with metol and iodine (Rao et al, 2003), sildenafil citrate also determined spectrophotometrically using p-chloranil and accelerated by hydrogen peroxide (Weinert et al, 2008), flow injection analysis (Altiokk et al, 2001), resonance ray lightscattering method (Liu et al, 2006), electro chemistry. (Othman et al, 2004 andHassan et al, 2006), electro spray tandem mass spectrometry (Abdel-Hamid 2006), high performance liquid chromatography (Daraghmeh et al, 2001;Tracqui et al, 2003 ;Nagaraju et al, 2003;Amar et al, 2011), and (HPTLC) (Ashutosh et al, 2012). In order to minimize batch -to-batch variation there is an immense need for developing a rapid, sensitive and validated analytical method for day-to-day analysis of the drug in pharmaceutical dosage forms.…”

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confidence: 99%

High Performance Liquid Chromatographic Method for Determination of Sildenafil Citrate (Viagra) in Pharmaceutical Formulation and Industrial Effluent Sample

Ahmed¹,

Lottfi²

2013

RJS

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A simple, precise, rapid and accurate reversed-phase high performance liquid chromatographic method has been developed for the determination of sildenafil citrate in a pure form, pharmaceutical formulations and industrial effluent samples. Chromatography was carried out on supelco L 7 reversed-phase column (25cm × 4.6mm), 5 microns, using a mixture of methanol: water: triethylamine (630: 370 :2 v/v/v) and adjusted to pH 4.0 with dilute phosphoric acid as a mobile phase at a flow rate of 1.0 ml.min-1 .Uv detection was performed at 220 nm at ambient temperature (25 °C). The retention time for sildenafil citrate found to be 4.6 minutes. The calibration curve was linear (r= 0.9998) over a concentration range from 10 to 70 µg/ml. Limit of detection (LOD) and limit of quantification (LOQ) were 60 ng/ml and 180 ng/ml respectively. The method was validated for its linearity, precision and accuracy. The proposed method was successfully applied to the determination of sildenafil citrate in tablets and industrial effluent samples.

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Separation and Determination of Synthetic Impurities of Sildenafil (Viagra) by Reversed-Phase High-Performance Liquid Chromatography

Cited by 24 publications

References 13 publications

Investigation of the Presence of Sildenafil in Herbal Dietary Supplements by Validated HPLC Method

Investigation of the Presence of Sildenafil in Herbal Dietary Supplements by Validated HPLC Method

Synthesis of core–shell magnetic molecularly imprinted polymers and detection of sildenafil and vardenafil in herbal dietary supplements

High Performance Liquid Chromatographic Method for Determination of Sildenafil Citrate (Viagra) in Pharmaceutical Formulation and Industrial Effluent Sample

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