scholarly journals Dietary Risk Assessment and Ranking of Multipesticides in Dendrobium officinale

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Meng-Ying Gu ◽  
Peng-Si Wang ◽  
Shang-Mei Shi ◽  
Jian Xue
Keyword(s):  
Pesticide Residues ◽  
High Performance ◽  
Hazard Quotient ◽  
Dietary Exposure ◽  
Dendrobium Officinale ◽  
Detection Frequency ◽  
Ranking Scheme ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Cumulative Risks

The presence of pesticide residues in Dendrobium officinale (D. officinale), a commonly used herbal medicine, has attracted much attention in recent years. Therefore, this study presents the levels of 141 pesticide residues in forty D. officinale samples, which were measured by high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). And we used a deterministic estimate model to assess chronic and acute dietary exposure risk, as well as the cumulative risks for adults, children, and specific groups of consumers. Furthermore, the residual risk of individual pesticides was sorted by adapting the matrix-ranking scheme. In 92.5% of the samples, 43 pesticides were detected, of which difenoconazole had the highest detection frequency. Multiple residues were detected in 85.0% of the samples, and one sample contained even up to 17 pesticides. The chronic hazard quotient (HQc) and the acute hazard quotient (HQa) were far below 100%, and both cumulative chronic and acute hazard indices (HI) did not exceed 100%. The risk scoring scheme showed that four pesticides were considered to pose a comparatively potential high risk, including difenoconazole, carbofuran, fipronil, and emamectin benzoate. The results indicated that the occurrence of pesticide residues in D. officinale could not pose a serious health problem to the public.

scholarly journals Simplified and Rapid Determination of Primaquine and 5,6-Orthoquinone Primaquine by UHPLC-MS/MS: Its Application to a Pharmacokinetic Study

Molecules ◽  
2021 ◽  
Vol 26 (14) ◽  
pp. 4357
Author(s):  
Waritda Pookmanee ◽  
Siriwan Thongthip ◽  
Jeeranut Tankanitlert ◽  
Mathirut Mungthin ◽  
Chonlaphat Sukasem ◽  
...  
Keyword(s):  
Pharmacokinetic Study ◽  
High Performance ◽  
Rapid Determination ◽  
Active Metabolites ◽  
Chromatography Tandem Mass Spectrometry ◽  
Accuracy And Precision ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Isocratic Mode

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.

scholarly journals Development and Validation of a Sensitive, Specific and Reproducible UPLC-MS/MS Method for the Quantification of OJT007, A Novel Anti-Leishmanial Agent: Application to a Pharmacokinetic Study

2021 ◽  
Vol 18 (9) ◽  
pp. 4624
Author(s):  
Maria Rincon Nigro ◽  
Jing Ma ◽  
Ololade Tosin Awosemo ◽  
Huan Xie ◽  
Omonike Arike Olaleye ◽  
...  
Keyword(s):  
Formic Acid ◽  
High Performance ◽  
Leishmania Major ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Positive Mode ◽  
Acquity Uplc

OJT007 is a methionine aminopeptidase 1 (MetAP1) inhibitor with potent anti-proliferative effects against Leishmania Major. In order to study its pharmacokinetics as a part of the drug development process, a sensitive, specific, and reproducible ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed and validated. Voriconazole was used as the internal standard to generate standard curves ranging from 5 to 1000 ng/mL. The separation was achieved using a UPLC system equipped with an Acquity UPLC BEH C18 column (2.1 × 50 mm, 1.7 μm) with 0.1% formic acid in acetonitrile and 0.1% formic acid in water as the mobile phase under gradient elution at a flow rate of 0.4 mL/min. The mass analysis was performed with a 4000 QTRAP® mass spectrometer using multiple-ion reaction monitoring (MRM) in the positive mode, with the transition of m/z 325 → m/z 205 for OJT007 and m/z 350 → m/z 101 for voriconazole. The intra- and inter-day precision and accuracy were within ±15%. The mean extraction recovery and the matrix effect were 95.1% and 7.96%, respectively, suggesting no significant matrix interfering with the quantification of the drug in rat plasma. This study was successfully used for the pharmacokinetic evaluation of OJT007 using the rat as an animal model.

scholarly journals Development and validation of a rapid UHPLC-MS/MS method for the determination of fenofibric acid in human plasma: Application to a pharmacokinetic study of fenofibrate tablet in Chinese subjects

2020 ◽  
Author(s):  
Xiaorong Wu ◽  
Yankai Wang ◽  
Binbin Liang ◽  
Honghai Wu ◽  
Liying Wu ◽  
...  
Keyword(s):  
Human Plasma ◽  
Pharmacokinetic Study ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Fenofibric Acid ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Development And Validation ◽  
Chinese Subjects

AbstractAn ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS) method was developed to determine the fenofibric acid (FA) in human plasma and applied to a pharmacokinetic study of fenofibrate tablet (Lipanthyl® supra, 160 mg) on Chinese subjects which had not been reported. Bezafibrate was used as an internal standard (IS), and the plasma samples were precipitated by methanol. Multiple reaction monitoring (MRM) mode was used to quantitatively analyzed FA m/z 317.2 → 230.7 and the IS m/z 360.0 → 274.0 in the electrospray ionization (ESI) negative interface. The calibration curves were linear over the range of 50–30,000  ng/mL (r2  ≥  0.996). The intra-day and inter-day precision (coefficient of variation, CV%) was less than 2.7 and 2.5%, respectively. The accuracy (relative error, RE%) ranged from −4.5 to 6.9%. The average recovery was higher than 86.2%, and the matrix effect was between 95.32 and 110.55%. The simple, rapid, and selectivity method was successfully applied to the pharmacokinetic study of fenofibrate tablets on Chinese subjects.

scholarly journals Development and Validation of a UPLC-MS/MS Method for the Quantitative Determination and Pharmacokinetic Analysis of Cirsimarin in Rat Plasma

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
En Zhang ◽  
Ying Wang ◽  
Fuyi Xie ◽  
Xinlei Zhuang ◽  
Xianqin Wang ◽  
...  
Keyword(s):  
Intravenous Administration ◽  
High Performance ◽  
Rat Plasma ◽  
Biological Properties ◽  
Pharmacokinetic Analysis ◽  
Standard Curve ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Development And Validation

Cirsimarin is a bioactive antilipogenic flavonoid isolated from the cotyledons of Abrus precatorius and represents one of the most abundant flavonoids present in this plant species. Cirsimarin exhibits excellent antioxidant, lipolysis, and other biological properties; it can effectively trigger lipid movement and demonstrates antiobesity effects. In this work, an ultra-high-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method was developed for the determination of cirsimarin in rat plasma after intravenous administration. A standard curve of cirsimarin in blank rat plasma was generated over the concentration range of 1–3000 ng/mL. Six rats were administered cirsimarin intravenously (1 mg/kg). The method only required 50 μL of plasma for sample preparation, and the plasma proteins were precipitated with acetonitrile to pretreat the plasma sample. The precisions of cirsimarin in rat plasma were less than 14%, while the accuracies varied between 92.5% and 107.3%. In addition, the matrix effect varied between 103.6% and 107.4%, while the recoveries were greater than 84.2%. This UPLC-MS/MS method was then applied in measuring the pharmacokinetics of cirsimarin in rats. The AUC(0-t) values of cirsimarin from the pharmacokinetic analysis were 1068.2 ± 359.2  ng/mL·h for intravenous administration. The half-life ( t 1 / 2 ) was 1.1 ± 0.4  h (intravenous), indicating that the metabolism of the compound was quick in the rats. Exploring the pharmacokinetics of cirsimarin in vivo can help better understand its metabolism.

scholarly journals The Effect of Tanreqing Injection on the Pharmacokinetics of Sirolimus in Rats

2019 ◽  
Vol 2019 ◽  
pp. 1-7 ◽  
Author(s):  
Feng Zhang ◽  
Liang Sun ◽  
Jianxiu Zhai ◽  
Tianyi Xia ◽  
Wei Jiang ◽  
...  
Keyword(s):  
High Performance ◽  
Room Temperature ◽  
Matrix Effects ◽  
Thaw Cycle ◽  
Relative Standard ◽  
The Matrix ◽  
Freeze Thaw Cycle ◽  
Liquid Chromatography Tandem Mass ◽  
The Stability ◽  
First Time

To evaluate the effect of Tanreqing injection on the pharmacokinetics of sirolimus in rats, a high performance liquid chromatography tandem mass spectrometry method was developed for sirolimus assay in whole blood. Calibration curve of sirolimus was acquired over a concentration ranging from 2.5 to 100 ng/mL with r2= 0.9955. The matrix effects and extraction recoveries of sirolimus ranged from 144% to 152% and from 80% to 96%, respectively. The inter- and intraday relative standard deviations were both <10%. The stability investigation showed that the blood samples were stable for 30-day-storage at -20°C, for 8 h storage at room temperature, for 24 h storage in the auto-sampler at 4°C, and for three freeze-thaw cycle process. The pharmacokinetic results demonstrated that the Cmax, AUC, and AUMC of sirolimus in rats (7.5 mg/kg, i.g.) were increased after beincoadministration with Tanreqing Injection at 2.5, 5.0, and 7.5 mL/kg (i.v.), respectively, or at 5 min, 2 h, and 4 h (5.0 mL/kg, i.v.) after SRL dosing, respectively. For the first time, the results proved the herb-drug interaction between Tanreqing Injection and sirolimus and accordingly suggested avoiding concurrent reception of those two drugs for patients.

scholarly journals Detecção de Resíduos de Agrotóxicos no Mel de Abelha

2014 ◽  
Vol 2 (2) ◽  
pp. 17
Author(s):  
F. M. Silva ◽  
D. C. Coelho ◽  
A. V. Machado ◽  
R. O. Costa
Keyword(s):  
Gas Chromatography ◽  
Liquid Chromatography ◽  
Pesticide Residues ◽  
High Performance ◽  
Solid Phase ◽  
Foreign Market ◽  
Extraction Methods ◽  
Uv Detector ◽  
Residue Detection ◽  
The Matrix

<p>As abelhas A. melífera são uns dos mais importantes polinizadores de culturas, além disso, elas produzem mel, própolis, geleia real e cera. O mel, principal produto da atividade apícola, utilizado como alimento, adoçante e para fins terapêuticos (apiterapia), tem a imagem de ser natural, saudável e limpo sendo esse um produto muito valorizado no mercado externo por isso, a busca por rigorosos padrões de qualidade se torna necessária para atender a um mercado consumidor cada vez mais exigente. Dessa forma a identificação da origem floral e geográfica, a ocorrência de adulterações e as contaminações, principalmente com antibióticos e agrotóxicos no mel tem se tornado uma rota importante devido os quais podem acarretar problemas de saúde ao consumidor. A dispersão da matriz em fase sólida (MSPD) combinada às técnicas cromatográficas modernas como cromatografia a gás (GC) e cromatografia a líquido (HPLC) é uma alternativa para evitar os diversos inconvenientes encontrados nos métodos clássicos de extração. A proposta desse trabalho foi pesquisar os diferentes tipos de Análises e metodologias de detecção de resíduos de agrotóxicos no mel de abelha Apresentando diferentes metodologias para a execução de estudos para validação de metodologia em métodos analítico, utilizando as técnicas de dispersão da matriz em fase sólida, cromatografia a gás acoplada à espectrometria de massas e cromatografia líquida de alta eficiência com detector espectrofotométrico com arranjo de diodos.</p><p><strong>Pesticide Residues in Honey Pesticide Residues detection in Bee honey</strong></p><pre> </pre><p><strong> </strong>A. mellifera bees are one of the most important pollinators of crops in addition they produce honey, propolis, royal jelly and wax. Honey, the main product of beekeeping, used as food, sweetener and in therapy (apitherapy), has the image of being natural, healthy and clean making a highly valued product in the foreign market so the search for rigorous standards of quality is needed to meet a consumer market increasingly demanding. Thus the identification of floral and geographical origin, the occurrence of tampering and contamination, especially with antibiotics and pesticides in honey has become an important route because which can cause health problems to consumers. The dispersion of the solid phase matrix (PDDM) combined with modern chromatographic techniques as gas chromatography (GC) and liquid chromatography (HPLC) is an alternative to avoid the various drawbacks found in classical extraction methods. The purpose of this study was to investigate the different types of analyzes and pesticide residue detection methodologies in honey Introducing different methodologies for carrying out studies for validation of a method in analytical methods, using the matrix dispersion techniques in solid phase, gas chromatography coupled to mass spectrometry and high-performance liquid chromatography with UV detector with diode array.</p>

scholarly journals Simultaneous Determination of Five Components of Chaihu-Shugan-San in Beagle Plasma by HPLC-MS/MS and Its Application to a Pharmacokinetic Study after a Single Dose of Chaihu-Shugan-San

2020 ◽  
Vol 2020 ◽  
pp. 1-11
Author(s):  
Yong-liang Zhu ◽  
Hui-jun Wang ◽  
Hao Xue ◽  
Yi Zhang ◽  
Qian-shi Cheng ◽  
...  
Keyword(s):  
Single Dose ◽  
High Performance ◽  
Matrix Effects ◽  
Gradient Elution ◽  
Gastrointestinal Diseases ◽  
Column Temperature ◽  
Mobile Phases ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Total Measurement Time

Chaihu-shugan-san (CHSGS) has been widely used in China to treat depression and gastrointestinal diseases for thousands of years, but little is known about its pharmacokinetic properties. The purpose of our study is to develop a reliable and sensitive high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method to detect five components in beagle plasma and study their pharmacokinetic after oral administration of CHSGS in beagles. An Agilent C18 column (2.1 × 150 mm, 3.5 μm) was used to separate the analytes, and the column temperature was maintained at 40°C. A gradient elution procedure was used with solvent A (acetonitrile) and solvent B (0.1% formic acid, aqueous) as mobile phases. The elution procedure was 60% B—10% B (0–3 min) and 10% B—60% B (3.1–4 min). The flow rate was 0.3 mL/min, and the total measurement time was 4 min. Within the determined range, the standard calibration curves of the five analytes had a satisfactory linear relationship (r2 ≥ 0.9923). The recovery rate (n = 6) of the five analytes was between 85.42% and 90.85%, and the matrix effects (n = 6) were between 94.52% and 103.91%. These results show that the validated method could be successfully applied to study the pharmacokinetic in beagles after a single dose of CHSGS.

scholarly journals A rapid, simultaneous and quantitative analysis of 26 ginsenosides in white and red Panax ginseng using LC–MS/MS

2021 ◽  
Vol 64 (1) ◽  
Author(s):  
Junghak Lee ◽  
Heeju Han ◽  
Xiu Yuan ◽  
Eunyoung Park ◽  
Jonghwa Lee ◽  
...  
Keyword(s):  
Quantitative Analysis ◽  
Panax Ginseng ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Standard Addition ◽  
Ginseng Extract ◽  
Quantitative Metabolomics ◽  
The Matrix ◽  
Metabolomics Study ◽  
Liquid Chromatography Tandem Mass

AbstractA quantitative analysis of ginsenoside is very important for ginseng studies because each ginsenoside shows different medical activity and metabolic pathway. In this study, a rapid, simultaneous, and quantitative analysis of 26 ginsenosides (Rb1, Rb2, Rc, Rd, Re, Rf, Rg1, Rg2(R), Rg2(S), Rg3(S), Rg3(R), Rg5, Rg6, Rh1(R), Rh1(S), Rh2(R), Rh2(S), F1, F2, F3, F4, K, Mc, PPT(S), XVII, and Y) in white, and red Panax ginseng was established using multiple reaction monitoring (MRM) mode on ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC–MS/MS). The mobile phase of water and methanol containing 0.1% formic acid and HSS T3 C18 analytical column was used for the chromatographic separation. The four sets of stereoisomers were successfully separated within a 26-min run time, eluting the S-isomer faster than the R-isomer with higher concentration. The ginseng extract was diluted by 100, 400 and 8000 times to fit in the calibration range and quantitated by the standard addition method. Matrix matched calibration by mixing 64 µL of the ginseng extract with 16 µL of the standard solution was used for compensating the matrix effect. Such quantitation methodology using dilution, standard addition and matrix matching resulted in precise and unambiguous quantitation of 26 ginsenosides in ginseng products. Major ginsenosides were observed at relatively higher concentrations in red Panax ginseng and the Mc was detected and quantitated for the first time in this study. The comprehensive quantitation system established in this study will contribute to quality evaluation, breeding and culturing, and quantitative metabolomics study of ginseng.

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