scholarly journals Quantitative Content Parameter in the Standardization of Veratrum Aqua, Veratrum Lobelianum Bernh. Based Drug

2021 ◽  
Vol 10 (1) ◽  
pp. 107-113
Author(s):  
E. V. Melnik ◽  
M. V. Belova ◽  
I. A. Tyurin ◽  
G. V. Ramenskaya

Introduction. According to the XIV Edition of the Russian Federation State Pharmacopoeia, the quality control of the «Veratrum Lobelianum rhizome and roots» herbal substance is carried out through the determination of the alkaloid sum by means of the titration-based method. There are no selective and sensitive instrumental methods for the quantitative analysis of veratrum aqua active ingredients either. Veratrum aqua is produced from the mentioned above herbal substance. Therefore, the study of veratrum aqua alkaloid composition is relevant, as well as the development of a modern analytical method for individual alkaloid determination that can be implemented in veratrum aqua standardization.Aim. To develop an approach to the quantitative analysis in Veratrum Aqua standardization.Materials and methods. Two analytical methods were developed: one for the veratrum alkaloid determination in veratrum aqua samples by means of high performance liquid chromatography coupled with tandem mass-spectrometry (HPLC-MS/MS), another – for jervine, the main veratrum aqua alkaloid, quantitation by means of HPLC with diode-array detector (HPLC-DAD).Results and discussion. Three main alkaloids, namely jervine, protoveratrine A and protoveratrine B, were identified in veratrum aqua. Jervine was found to be the most abundant one, hence it was chosen for the further development of a more affordable HPLC-DAD method. This method was validated for specificity, linearity, accuracy and precision. Jervine concentrations were measured in seven veratrum aqua samples produced by different manufacturers.Conclusion. The highest jervine concentration among the examined samples was found to be 170 µg/ml, the lowest – 136 µg/ml. It is proposed to implement the following quantitative content parameter in veratrum aqua standardization: «Quantitative test. Jervine content should be not lessthan 136 µg/ml». This parameter is to be determined by HPLC-DAD.

2010 ◽  
Vol 5 (1) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Wen-Yuan Liu ◽  
Feng Feng ◽  
Cheng-Xia Yu ◽  
Ning Xie

A sensitive and selective high performance liquid chromatographic method coupled with DAD detection is presented for quality control of Radix Ilicis Pubescentis. By means of this analytical procedure the major individual constituents (ilexoside O, ilexgenin A, ilexsaponin A1, ilexsaponin B1, liriodendin and acanthoside B) could be quantified simultaneously. LC-ESIMS was applied for identification of the six compounds in the plant by comparing their m/z value and retention times with those of selected standards. For quantitative analysis, the extraction procedure and the extraction solvent were optimized in order to ensure the exhaustive extraction of the plant material. The HPLC conditions were evaluated and optimized for the exact quantification of all six individual compounds. Chromatographic separation was carried out on a C18 column using gradient elution with acetonitrile and 0.1% phosphoric acid as the mobile phase. Detection was carried out using a photodiode array detector. The calibration curves for determination of the six constituents showed good linearity over the investigated ranges (r2>0.999). Measurement of intra-day and inter-day variability (expressed as RSD value) was conducted to assess precisions of the method, and RSD (%) of intra- and inter-day variation were between 1.56-3.36% and 1.61-3.58%, respectively. The recoveries of the six compounds were between 96.4-102.2%, with RSD (%) values ranging from 1.7-3.8%. These validation results demonstrated the suitability of the method for the precise and accurate determination of the main constituents in Radix Ilicis Pubescentis. The method was successfully applied for quality evaluation of 12 batches of Radix Ilicis Pubescentis obtained from different regions of southern China. The contents of the six major constituents varied significantly due to their different origins, which can be used as an aid to assessing the quality of Radix Ilicis Pubescentis.


2020 ◽  
Vol 23 (10) ◽  
pp. 1010-1022
Author(s):  
Emrah Dural

Aim and scope: Due to the serious toxicological risks and their widespread use, quantitative determination of phthalates in cosmetic products have importance for public health. The aim of this study was to develop a validated simple, rapid and reliable high-performance liquid chromatography (HPLC) method for the determination of phthalates which are; dimethyl phthalate (DMP), diethyl phthalate (DEP), benzyl butyl phthalate (BBP), di-n-butyl phthalate (DBP), di(2- ethylhexyl) phthalate (DEHP), in cosmetic products and to investigate these phthalate (PHT) levels in 48 cosmetic products marketing in Sivas, Turkey. Materials and Methods: Separation was achieved by a reverse-phase ACE-5 C18 column (4.6 x 250 mm, 5.0 μm). As the mobile phase, 5 mM KH2PO4 and acetonitrile were used gradiently at 1.5 ml min-1. All PHT esters were detected at 230 nm and the run time was taking 21 minutes. Results: This method showed the high sensitivity value the limit of quantification (LOQ) values for which are below 0.64 μg mL-1 of all phthalates. Method linearity was ≥0.999 (r2). Accuracy and precision values of all phthalates were calculated between (-6.5) and 6.6 (RE%) and ≤6.2 (RSD%), respectively. Average recovery was between 94.8% and 99.6%. Forty-eight samples used for both babies and adults were successfully analyzed by the developed method. Results have shown that, DMP (340.7 μg mL-1 ±323.7), DEP (1852.1 μg mL-1 ± 2192.0), and DBP (691.3 μg mL-1 ± 1378.5) were used highly in nail polish, fragrance and cream products, respectively. Conclusion: Phthalate esters, which are mostly detected in the content of fragrance, cream and nail polish products and our research in general, are DEP (1852.1 μg mL-1 ± 2192.0), DBP (691.3 μg mL-1 ± 1378.5) and DMP (340.7 μg mL-1 ±323.7), respectively. Phthalates were found in the content of all 48 cosmetic products examined, and the most detected phthalates in general average were DEP (581.7 μg mL-1 + 1405.2) with a rate of 79.2%. The unexpectedly high phthalate content in the examined cosmetic products revealed a great risk of these products on human health. The developed method is a simple, sensitive, reliable and economical alternative for the determination of phthalates in the content of cosmetic products, it can be used to identify phthalate esters in different products after some modifications.


2020 ◽  
Vol 16 (6) ◽  
pp. 671-689
Author(s):  
Marcin Gackowski ◽  
Marcin Koba ◽  
Katarzyna Mądra-Gackowska ◽  
Piotr Kośliński ◽  
Stefan Kruszewski

At present, no one can imagine drug development, marketing and post-marketing without rigorous quality control at each stage. Only modern, selective, accurate and precise analytical methods for determination of active compounds, their degradation products and stability studies are able to assure the appropriate amount and purity of drugs administered every day to millions of patients all over the world. For routine control of drugs simple, economic, rapid and reliable methods are desirable. The major focus of current scrutiny is placed on high-performance thin layer chromatography and derivative spectrophotometry methods, which fulfill routine drug estimation’s expectations [1-4]. The present paper reveals state-of-the-art and possible applications of those methods in pharmaceutical analysis between 2010 and 2018. The review shows advantages of high-performance thin layer chromatography and derivative spectrophotometry, including accuracy and precision comparable to more expensive and time-consuming methods as well as additional fields of possible applications, which contribute to resolving many analytical problems in everyday laboratory practice.


2019 ◽  
Vol 15 (2) ◽  
pp. 130-137
Author(s):  
Hui Jiang ◽  
Lianhao Fu ◽  
Yu Wang ◽  
Shaozhi Wang ◽  
Xiaoxu Zhang ◽  
...  

Background: Jingzhiguanxin (JZGX) tablet, a traditional Chinese prescription, is commonly used for treating coronary heart disease and angina pectoris in the clinic. There are six active components (Danshensu (DSS), Protocatechuic aldehyde (PD), Paeoniflorin (PF), Ferulic acid (FA), Salvianolic acid B (Sal B) and Tanshinone IIA (TA)) in JZGX tablet. </P><P> Objective: In this paper, a simple and reliable method was used for simultaneous determining the six active components by high-performance liquid chromatography coupled with diode array detector (HPLC-DAD). Methods: These six active components were separated on an Agilent Zorbax Eclipse XDB-C18 column (150 mmx4.6 mm, 5 µm) at 30 °C. Acetonitrile (A), methanol (B) and 0.5% H3PO4 aqueous solution (C) were used as mobile phase for gradient elution. The flow rate was 1 mL/min and the detection wavelengths were set at 280 nm for DSS, PD and Sal B, 230 nm for PF, 320 nm for FA and 270 nm for TA, respectively. Results: All of the six components showed good linearity regressions (r2≥0.9997) in the detected concentration range. The recovery rates and coefficient of variation (CV) for all analytes were 98.66%- 100.18% and 0.75%-1.89%, respectively. This method was successfully applied to simultaneously determine the six components in JZGX tablet from different batches and manufacturers. Conclusion: The validated method can be used in routine quality control analysis of JZGX tablet without any interference.


Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  

The method for the determination of primaquine (PQ) and 5,6-orthoquinone primaquine (5,6-PQ), the representative marker for PQ active metabolites, via CYP2D6 in human plasma and urine has been validated. All samples were extracted using acetonitrile for protein precipitation and analyzed using the ultra-high-performance liquid chromatography–tandem mass spectrometry (UHPLC-MS/MS) system. Chromatography separation was carried out using a Hypersil GOLDTM aQ C18 column (100 × 2.1 mm, particle size 1.9 μm) with a C18 guard column (4 × 3 mm) flowed with an isocratic mode of methanol, water, and acetonitrile in an optimal ratio at 0.4 mL/min. The retention times of 5,6-PQ and PQ in plasma and urine were 0.8 and 1.6 min, respectively. The method was validated according to the guideline. The linearity of the analytes was in the range of 25–1500 ng/mL. The matrix effect of PQ and 5,6-PQ ranged from 100% to 116% and from 87% to 104% for plasma, and from 87% to 89% and from 86% to 87% for urine, respectively. The recovery of PQ and 5,6-PQ ranged from 78% to 95% and form 80% to 98% for plasma, and from 102% to from 112% to 97% to 109% for urine, respectively. The accuracy and precision of PQ and 5,6-PQ in plasma and urine were within the acceptance criteria. The samples should be kept in the freezer (−80 °C) and analyzed within 7 days due to the metabolite stability. This validated UHPLC-MS/MS method was beneficial for a pharmacokinetic study in subjects receiving PQ.


Marine Drugs ◽  
2021 ◽  
Vol 19 (6) ◽  
pp. 321
Author(s):  
Maria Orfanoudaki ◽  
Anja Hartmann ◽  
Julia Mayr ◽  
Félix L. Figueroa ◽  
Julia Vega ◽  
...  

This study presents the validation of a high-performance liquid chromatography diode array detector (HPLC-DAD) method for the determination of different mycosporine-like amino acids (MAAs) in the red alga Bostrychia scorpioides. The investigated MAAs, named bostrychines, have only been found in this specific species so far. The developed HPLC-DAD method was successfully applied for the quantification of the major MAAs in Bostrychia scorpioides extracts, collected from four different countries in Europe showing only minor differences between the investigated samples. In the past, several Bostrychia spp. have been reported to include cryptic species, and in some cases such as B. calliptera, B. simpliciuscula, and B. moritziana, the polyphyly was supported by differences in their MAA composition. The uniformity in the MAA composition of the investigated B. scorpioides samples is in agreement with the reported monophyly of this Bostrychia sp.


2016 ◽  
Vol 8 (30) ◽  
pp. 5949-5956 ◽  
Author(s):  
Soumia Boulahlib ◽  
Ali Boudina ◽  
Kahina Si-Ahmed ◽  
Yassine Bessekhouad ◽  
Mohamed Trari

In this study, a rapid and simple method based on reversed-phase high performance liquid chromatography (RP-HPLC) using a photodiode array detector (PDA) for the simultaneous analysis of five pollutants including aniline and its degradation products, para-aminophenol, meta-aminophenol, ortho-aminophenol and phenol, was developed.


Author(s):  
Xiaoyong Zhang ◽  
Xuezhao Chen ◽  
Juan Jin ◽  
Minghua Gong ◽  
Qiang He ◽  
...  

Abstract Capilliposide B (CPS-B) and Capilliposide C (CPS-C), as the key components in Lysimachia capillipes Hemsl., increasingly aroused the interest and research concern of many researchers due to the good bioactivities. Nowadays, the reference standards of CPS-B and CPS-C yield were very limited. Due to the deficit of reference standards, the determination could be difficult to carry out, and the quality control and evaluation would be restrained afterwards. To solve this urgent problem, a quantitative analysis of multi-components by single-marker (QAMS) method was proposed and established based on high-performance liquid-chromatography tandem evaporative light-scattering detector. In this QAMS method, the content of the two bioactive components could be calculated by buddlejasaponin IV, which is applied as an external standard and readily obtained. And the methodological experiments were evaluated and indicated accuracy, stability and feasibility of this QAMS method. Therefore, in this study, this built method would properly meet the requirement of determination of CPS-B, CPS-C and quality control of the L. capillipes Hemsl. plant.


2021 ◽  
Vol 32 (4) ◽  
pp. 867-873
Author(s):  
Helmy Yusuf ◽  
Nina Wijiani ◽  
Rizka Arifa Rahmawati ◽  
Riesta Primaharinastiti ◽  
M. Agus Syamsur Rijal ◽  
...  

Abstract Objectives Curcumin belongs to the family of curcuminoids, natural polyphenolic compounds that possesses neuroprotective properties, anti inflammatory and anticancer. Its entrapment in the developed casein-based micellar powder (CMP) and poloxamer-based micellar powder (PMP) was to enhance the solubility and improve the bioavailability. Henceforth, the present study aimed to acquire an efficient analytical method for the curcumin analysis in polymeric micellar formulations. Methods A fast and specific HPLC method was developed for analyzing curcumin in two different micellar matrices using casein and poloxamer. The HPLC was equipped with a C18 column (250 × 4 mm, 5 µm) and diode array detector. A designated isocratic elution of curcumin was employed using mobile phase with a composition of water (1%, v/v acetic acid) and acetonitrile in a ratio of 50:50 v/v. The employed flow rate was 1.0 mL/min and the analyte was examined at 421 nm. Results An effective analysis in HPLC was successfully achieved by the predetermined HPLC condition. A good resolution of peaks at the employed flow rate was achieved. The linearity was excellent in two different range of concentrations, 2–20 and 10–50 μg/mL. The selectivity, accuracy and precision fulfilled the acceptable requirements. Conclusions The developed method was practically effective to qualitatively identified curcumin. In addition, the assay also effectively quantified the amount of curcumin in the polymeric entrapping matrices which demonstrates that it has great potential to be used in natural compound analysis.


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