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Abstract

Flavonoids are the most abundant components in Salvia plebeia, with significant pharmacological antioxidant and hepatoprotective properties. Hispidulin and homoplantaginin are the main flavonoid components in S. Plebeia. In this study, we established an ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) to determine hispidulin and homoplantaginin in rat plasma samples, which were precipitated using acetonitrile-methanol (9:1, v/v). We used a UPLC HSS T3 (100 mm × 2.1 mm, 1.7 μm diameter) chromatographic column, an acetonitrile-water (containing 0.1% formic acid) mobile phase, and a gradient elution flow rate of 0.4 mL min−1 in an elution time of 4 min. We used electrospray ionization (ESI) detection in positive ion mode, and multiple reaction monitoring mode (MRM) for quantitative analysis: m/z 301 → 286 for hispidulin, m/z 463 → 301 for homoplantaginin, and m/z 465 → 303 for internal standard (IS). In pharmacokinetic studies, 24 rats were orally administered hispidulin and homoplantaginin (5 mg kg−1) and received sublingual intravenous injections (1 mg kg−1) at two different doses, four groups with six rats/group. Differences in hispidulin and homoplantaginin pharmacokinetics in rat plasma were evaluated. The calibration curve showed good linearity in the 0.5–1,000 ng mL−1 range, with r > 0.99. Precision, accuracy, recovery, matrix effects, and stability results all met standard biological sample detection requirements. Our pharmacokinetic studies showed hispidulin bioavailability was much higher than homoplantaginin at 17.8% and 0.1%, respectively.

Open access
Acta Chromatographica
Authors:
Waqar Siddique
,
Rai Muhammad Sarfraz
,
Muhammad Zaman
,
Riffat Khan
,
Maria Gul
,
Farhan Asghar
,
Tangina Malik
,
Asiya Saif
,
Qurat-Ul-Ain Shamim
,
Ahmad Salawi
,
Meshal Alshamrani
,
Yosif Almoshari
, and
Fahad Y. Sabei

Abstract

One of the most effective, rapid, and simple methods reversed-phase high-performance liquid chromatography (RP-HPLC) was used for simultaneous development and validation of Eletriptan hydrobromide (ELE HBR) and Itopride hydrochloride (ITP HCL) in combination. The method was validated based on the regulations of United States Pharmacopeia (USP) and International Conference on Harmonization (ICH) guidelines. Separation of both drugs was achieved within approximately 5 min by using a mobile phase made up of a 70:30 ratio of phosphate buffer and acetonitrile having a flow rate of 1 mL min−1. Furthermore, a comprehensive study was conducted on precision, accuracy, linearity, inter-day, intra-day studies, an assay of formulated films, and stability studies of combined prepared film. Co-efficient of correlation ranged between 0.9993, and 0.9965 for ELE HBR and ITP HCL respectively. The accuracy of the developed method was accurate as drug recoveries in both cases of ITP HCL, and ELE HBR falls between (99.87, 99.96, and 99.84%) to (99.81, 99.12, and 98.44%) respectively having a concentration range of solutions between 10, 30 and 50 μg mL−1 dilution. Films developed by using both drugs in combination were then validated for assay studies, and it was found that substantial results of 99.05%, and 99.87% were found in the case of ITP HCL and ELE HBR respectively. The stability of the solution and mobile phase showed the method's accuracy as the results were 97% for ITP HCL and 99% for ELE HBR. The proposed method developed for simultaneous determination of ITP HCL and ELE HBR was developed and validation and no interaction of any excipient were found.

Open access

Abstract

In this work, a simple and rapid high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) method was developed and validated to carry out the simultaneous measurement of busulfan (BU) and phenytoin (PHT) in the plasma of children. In this method, plasma sample could be prepared by one-step protein precipitation using 1 mL of methanol/water (1:1, v/v). After centrifugation (14,500 rpm, 5 min, 4 °C), 10 μL of the supernatant was injected into a Hypersil Gold C18 column (150 × 2.1 mm, 5 μm, Thermo Fisher Scientific) for separation by gradient elution. Quantification was carried out using multiple reactions monitoring (MRM) under positive scan mode. In the method verification, the calibration curves of BU and PHT showed satisfactory linearity (r > 0.99) at the concentration ranging from 0.02 to 20 μg mL−1. The accuracy and precision were tested at four concentration levels (including the LLOQ level) with the relative error (RE) ranging from −0.80% to 11.45% and coefficient of variation (CV) between 0.93% and 7.74%. There was no pronounced matrix effect to interfere with the quantitative analysis. Compared to determine BU and PHT using two individual methods, less pre-treatment process, labor and blood sample volume are required in this proposed method. Finally, this method was successfully applied to the therapeutic drug monitoring of BU and PHT for children underwent hematological stem cell transplantation.

Open access
Acta Chromatographica
Authors:
Tiantian Lu
,
Xiaohong Wang
,
Qi Zhang
,
Kun Liu
,
Tongxin Xu
,
Quande Wang
,
Pengfei Zhao
, and
Zhongzhe Cheng

Abstract

Solasodine, a steroidal alkaloid, is distributed extensively in Solanaceae plants with multiple biological activities such as neuroprotection, antineoplastic and anticonvulsant activities. However, there is little information about the excretion of intact solasodine in vivo. To investigate its excretion, a reliable LC-MS/MS method for quantitation solasodine in rat urine and feces was established and validated. Sample preparation was carried out by liquid-liquid extraction using MTBE as extractant. Moreover, rat urine was preconditioned with BSA, an anti-adsorptive additive, to prevent the nonspecific binding of solasodine to containers and tubes. The method was validated over the range of 4–2000 ng mL−1. The correlation coefficient (r 2) were all above 0.999. The intra- and inter-day precision and accuracy were within 16.9% and between −11.0 and 8.9%, respectively. The recovery of solasodine in urine and feces was in the range of 72.5–80.3 and 75.7–80.2%, respectively. IS-normalized matrix factor ranged from 0.94 to 1.12 with RSD% ≤4.02%. This method was successfully applied to the excretion study of solasodine following oral and intravenous administration.

Open access

Abstract

A new pretreatment method termed ultrasound-assisted extraction (UAE) which is combined with solid-phase extraction which is combined with dispersive liquid-liquid microextraction (SPE-DLLME) followed by gas chromatography-flame ionization detector (GC-FID) analysis has been developed for the determination of diazinon in garden parsley as vegetable samples. The analyte was extracted from garden parsley sample using ultrasound-assisted extraction followed by solid-phase extraction followed by dispersive liquid-liquid microextraction. Various parameters that affect the efficiency of the extraction techniques have been optimized. The calibration plot was linear in the range of 5.0–1,000 μg kg−1 with detection limit of 1.0 μg kg−1 for diazinon in garden parsley samples. The results confirm the suitability of the UAE-SPE-DLLME-GC-FID as a sensitive method for the analysis of the targeted analyte in garden parsley samples.

Open access

Abstract

Fuke Yangrong pill, a traditional Chinese patent medicine, with the functions of nourishing qi and blood, soothing liver and relieving depression, regulating menstruation and removing blood stasis, is composed of 16 Chinese medicinal herbs. For quality control purpose, an HPLC method was established for simultaneous quantification of paeoniflorin, hesperidin and ligustilide in Fuke Yangrong pill. With acetonitrile-0.1% formic acid as mobile phase, gradient elution was carried out using Agilent ZORBAX Eclipse Plus C18 column (250 mm × 4.6 mm, 5.0 μm) at 1.0 mL min−1. Detection wavelength was set at 230 nm for paeoniflorin, 280 nm for hesperidin and ligustilide. The temperature was 30 °C. There was a good linearity between the peak area and the concentration of each component to be measured within their linear range (r ≥ 0.9994). The average recoveries were between 98.6% and 102.6% with RSDs no more than 2.93%. This method was validated to be accurate and convenient, which is suitable for the quality control of Fuke Yangrong pill.

Open access

Abstract

In this study, an accurate, simple, economical and precise Reversed-Phase High Pressure Liquid Chromatography (RP-HPLC) method was developed for the simultaneous estimation of Ozenoxacin and Benzoic Acid in a pharmaceutical cream formulation, according to the International Conference on Harmonisation (ICH) guidelines. Chromatographic separation was achieved by gradient elution, on RP-HPLC Instrument, equipped with column C8 (150 mm × 4.6 mm, 5 μm particle size) using Ultra Violet (UV) detector at 235 nm wavelength, by using Mobile Phase A: triethylamine, trifloroacetic acid and water (1:1:1000) and Mobile Phase B: methanol and Diluent: water, acetonitrile and triethylamine (500:500:1), at flow rate 0.8 mL min−1; injection volume of 20 μL; column oven temperature 45 °C and sample temperature: 25 °C; Run time: 15 min. All the validation parameters were within the acceptance criteria, as per ICH requirements, for Ozenoxacin and Benzoic acid. Consequently, this method has found to be validated, simple, rapid and successfully applicable, to the simultaneous estimation of Ozenoxacin and Benzoic acid by RP-HPLC, for routine analytical testing in quality control, with a run time of 15 min and for future research studies. Forced degradation of Ozenoxacin cream 1% w/w formulation was performed and found that validated method has stability indicating potential that needs to be further studied.

Open access

Abstract

Food, water, and energy scarcity threaten India's future, and they must be addressed first. To meet the country's ever-increasing population needs, agricultural productivity must be expanded. For the crop-land suitability, we have studied an area of about 6,539 km2 in Vizianagaram district. The majority of the land is used for paddy agriculture (Kharif). The crop-land suitability has been evaluated based on the different parameters identified in that study area. “Remote sensing (RS)” and “geographic information system (GIS)” were combined for the crop-land suitability using nine parameters. The slope, elevation, rainfall, soil texture, lithology, groundwater, land use–land cover (LULC), TWI, and land surface temperature are the primary criteria used to determine the crop-land suitability in the Vizianagaram district (AP). Thematic maps were created using Landsat 8 images and SRTM DEM images from USGS Earth Explorer. Based on these maps and the influence of these parameters, we may assign weights to the parameters and then rank them, the Analytic Hierarchy Process (AHP) allowing us to identify which area is more suitable for good crop productivity and which is not. In this study, the soils are divided into four categories: low suitability, moderate suitability, high suitability, and extremely high suitability. The suitability index is found to be in the range of 0–55.2%, which indicates the lack of outstanding agricultural lands in the sudy region.

Restricted access