scholarly journals Development and Application of an UHPLC-MS/MS Method for Comparative Pharmacokinetic Study of Eight Major Bioactive Components from Yin Chen Hao Tang in Normal and Acute Liver Injured Rats

2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Yun Wang ◽  
Xinrui Xing ◽  
Yan Cao ◽  
Liang Zhao ◽  
Sen Sun ◽  
...  
Keyword(s):  
Lower Limit ◽  
Limit Of Detection ◽  
Injury Model ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Bioactive Ingredients ◽  
Aloe Emodin ◽  
Plasma Pharmacokinetics ◽  
Ultrahigh Performance Liquid Chromatography

Yin Chen Hao Tang (YCHT) is one of the most famous hepatoprotective herbal formulas in China, but its pharmacokinetic investigation in model rats has been rarely conducted. In this study, the hepatic injury model was caused by intraperitoneal injections of carbon tetrachloride (CCl4), and YCHT was orally administered to the model and normal rats. An ultrahigh performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method was established to analyze the plasma pharmacokinetics of eight major bioactive ingredients from YCHT in both the normal and liver injured rats. The calibration curves presented good linearity (r > 0.9981) in the concentration range. The relative standard deviation (RSD%) of inter- and intraday precision was within 9.55%, and the accuracy (RE%) ranged from -10.72% to 2.46%. The extraction recovery, matrix effect, and stability were demonstrated to be within acceptable ranges. The lower limit of detection (LLOD) and lower limit of quantitation (LLOQ) were around 0.1 ng/mL and 0.5 ng/mL, respectively, which were much lower than those in other related researches. Results reveal that there are significant differences in the pharmacokinetics of scoparone, geniposide, rhein, aloe-emodin, physcion, and chrysophanol in hepatic injured rats as compared to those in control except for scopoletin and emodin. Our experimental results provide a meaningful reference for the clinical dosage of YCHT in treating liver disorders, and the improvement of LLOD and LLOQ can also broaden the range of our method’s application, which is very suitable for quantitating these eight compounds with low levels.

scholarly journals Residues, degradation behavior of cyproconazole in Sichuan pepper and its dietary risk assessment

2021 ◽  
Author(s):  
Feng Xu ◽  
Wenhao Ren ◽  
Duo Xu ◽  
Ying Qu ◽  
Juanfei Qi ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Hazard Quotient ◽  
Hazard Index ◽  
Maximum Residue Limit ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Ultrahigh Performance Liquid Chromatography ◽  
Dietary Risk Assessment

Abstract In this study, an efficient method was developed and validated to determine cyproconazole in Sichuan pepper samples using the QuEChERS procedure and ultrahigh-performance liquid chromatography-tandem mass spectrometry. The average recoveries of the method were 96.2%-104.5% with the relative standard deviation (RSDs) below 7.6%, the limit of detection (LOD), and the limit of quantitation (LOQ) was 0.001 mg/kg and 0.02 mg/kg. The field trial results showed that cyproconazole in two Sichuan pepper matrices was rapidly dissipated with half-lives less than 8.8 days, which could be regarded as an easy degradation pesticide. The terminal residues of cyproconazole in Sichuan pepper samples were lower than the maximum residue limit (MRL) set by China (0.2 mg/kg registered on wheat). The calculated hazard quotient and acute hazard index lower than 100% illustrated that the use of cyproconazole, even at 1.5 times the highest recommended dose, does not pose any hazards to consumers.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

A Selective and Sensitive Method Development and Validation of 1,1-Dimethyl-3-Hydroxy-Pyrrolidinium Bromide Impurity in Glycopyrrolate Oral Solution by Liquid Chromatography–Tandem Mass Spectroscopy

2021 ◽  
Author(s):  
Rajesh Kumar Chawla ◽  
G S N Koteswara Rao ◽  
Umasankar Kulandaivelu ◽  
Siva Prasad Panda ◽  
Rajasekhar Reddy Alavala
Keyword(s):  
Liquid Chromatography ◽  
Mobile Phase ◽  
Method Development ◽  
Limit Of Detection ◽  
Oral Solution ◽  
Calibration Plot ◽  
Tandem Mass ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Abstract Objective A selective and sensitive liquid chromatography–tandem mass spectrometer (LC–MS/MS) method has been developed for the quantification of 1,1-dimethyl-3-hydroxy-pyrrolidinium bromide impurity in glycopyrrolate oral solution. Materials and method The LC–MS/MS analysis was done on X Bridge HILIC (100 × 4.6 mm, 5 μm) analytical column, and the mobile phase used was10 mM ammonium formate with 0.2% formic acid as mobile phase-A and acetonitrile as mobile phase-B with a gradient programme of 5.0 min. The flow rate used was 1.2 mL/min. Triple quadrupole mass detector coupled to positive electrospray ionization operated in multiple reactions monitoring mode was used for the quantification at m/z 116.10 ± 0.5. Results Retention time of impurity was found ~3.2 min. The method was validated in terms of specificity, linearity, accuracy, precision, range, limit of detection, limit of quantitation (LOQ) and robustness. Relative standard deviation (RSD) for system suitability was found 1.3%. Calibration plot was linear over the range of 0.050–2.000 μg/mL. Limit of detection and limit of quantification were found 0.017 and 0.051 μg/mL, respectively. The intra- and inter-day precision RSD was 2.3% and the obtained recovery at LOQ to 200% was in between 86.7 and 107.4%. Conclusion The low RSD values and high recoveries of the method confirm the suitability of the method.

Concentrations of Bisphenols in Canned Foods and Their Risk Assessment in Korea

2018 ◽  
Vol 81 (6) ◽  
pp. 903-916 ◽  
Author(s):  
SU JEONG CHOI ◽  
EUN SUN YUN ◽  
JAE MIN SHIN ◽  
YEO SOOK KIM ◽  
JEONG SOOK LEE ◽  
...  
Keyword(s):  
Body Weight ◽  
Limit Of Detection ◽  
Daily Intake ◽  
Correlation Coefficients ◽  
Dietary Exposure ◽  
Related Risk ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass ◽  
Canned Foods

ABSTRACT The purpose of this study was to survey concentrations of bisphenols in canned foods using liquid chromatography–tandem mass spectrometry, to estimate the dietary exposure to bisphenols, and to assess the related risk for the Korean population from the intake of canned foods. The linearity of bisphenols in the range of 2.5 to 725 μg/L was satisfactory with correlation coefficients (r2) of 0.999. The limit of detection was 0.14 to 5.85 μg/L, and the limit of quantitation was 0.44 to 17.73 μg/L. Sample recoveries were 70.56 to 113.6%, with relative standard deviations below 10% for spiking levels of 50 and 250 μg/kg (15 and 75 μg/kg for BPS). The bisphenol concentrations in 104 canned foods ranged from undetectable to 1,525 μg/kg. The estimated mean daily intake of bisphenols was 0.54 to 78.69 ng/kg of body weight per day, and the 95th percentile daily intake was 1.92 to 134 ng/kg of body weight per day. Therefore, the intake of bisphenols from canned foods for the population in Korea is unlikely to cause human health problems. The analytical methods used are suitable for regular monitoring and assessment of human exposure to bisphenols from foods.

scholarly journals Development and Validation of RP-HPLC Method for Ziprasidone Hydrochloride Monohydrate

2016 ◽  
Vol 8 (02) ◽  
Author(s):  
Abhay R. Shirode ◽  
Arpita Nath ◽  
Vilasrao Kadam
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Rp Hplc ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Water Ph ◽  
Hydrochloride Monohydrate

A new isocratic simple and rapid reverse phase high performance liquid chromatographic (RP-HPLC) method was developed and successively validated for the estimation of ziprasidone hydrochloride monohydrate (ZHM). In this newly developed method chromatographic separation of ZHM was achieved on a Hemochrom-Intertsil C18-5U column (250 × 4.6) mm within a short runtime of 6.5min using mobile phase containing HPLC grade water (pH adjusted to 3.0 with glacial acetic acid AR) and methanol in the ratio of 45:55% v/v. ZHM was estimated with UV detection at 317nm and it was found to be eluted at 4.8min. The above mentioned method was validated as per International Conference on Harmonization (ICH) guidelines with respect to accuracy, precision, linearity, lower limit of detection (LOD) and lower limit of quantitation (LOQ) and robustness. The method was found specific for ZHM and linear (r2 =0.998) over concentrations ranging from 2 to12μg/ml. The method was found statically accurate (mean recovery = 100.46%), precise with both intra-day and inter-day relative standard deviation (RSD) values less than 1.0% and robust. The obtained results concluded that the proposed RP-HPLC method is convenient, reliable and useful in routine analysis for estimation of ZHM in its bulk form and dosage form.

Rapid and Sensitive Liquid Chromatographic Method for Determination of Anastrozole in Different Polymer–Lipid Hybrid Nanoparticles

2021 ◽  
pp. 247263032098230
Author(s):  
Dilshad Ahmad ◽  
Faisal A. Al Meshaiti ◽  
Yazeed K. Al Anazi ◽  
Osama Al Owassil ◽  
Alaa Eldeen B. Yassin
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Hplc Method ◽  
Hybrid Nanoparticles ◽  
Array Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Inhibitor Drug

Anastrozole, an aromatase inhibitor drug, is used for the treatment of breast cancer in pre- and postmenopausal women. Anastrozole’s incorporation into nanoparticulate carriers would enhance its therapeutic performance. To perceive the exact loaded amount of drug in nanocarriers, a valid analytical method is required. The reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated by using the C18 column, 150 × 4.6 mm, 5 µm particle size, in isocratic mobile phase composed of 50:50 V/V (volume/volume) acetonitrile–phosphate buffer (pH 3) flowing at a rate of 1.0 mL/min, and a diode array detector (DAD) set at λmax = 215 nm. The validation parameters such as linearity, accuracy, specificity, precision, and robustness have proven the accuracy of the method, with the relative standard deviation percentage (% RSD) values < 2. The limit of detection of the method was found equal to 0.0150 µg/mL, and the limit of quantitation was 0.0607 µg/mL. The percent recovery of sample was in the range of 98.04–99.25%. The method has the advantage of being rapid with a drug retention time of 2.767 min, specific in terms of resolution of peaks void of interference with any of the excipients, and high reproducibility. This makes it highly applicable for quality control purposes.

Simultaneous Determination of Four Herbicide and Pesticide Residues in Chinese Green Tea Using QuEChERS Purification Procedure and UPLC-MS/MS Analysis

2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Green Tea ◽  
Limit Of Detection ◽  
Multiple Reaction Monitoring ◽  
Graphitized Carbon Black ◽  
Ms Analysis ◽  
Relative Standard ◽  
Limit Of Quantitation

A method for simultaneous determination of residuals of four herbicides and pesticides, simazine, carboxin, diflubenzuron and rotenone, in Chinese green tea was developed. In the proposed method, the tea powder was placed in a centrifuge tube with a plug, extracted in saturated aqueous sodium chloride solution and acetonitrile, agitated using vortex oscillator, and then centrifuged 5 min at 4000 rpm. The supernatant solution was purified by primary secondary amine (PSA) sorbent, C18 power, and graphitized carbon black powder, respectively. Then the purified extracts were dissolved with acetonitrile:0.1% formic acid aqueous solution (40:60, V/V) and agitated, filtered using a syringe with 0.22 μm nylon filter prior to UPLC-MS/MS analysis. The UPLC analysis was performed on an ACQUITY UPLC® HSS T3 column (2.1 mm×100 mm, 1.8 µm), using acetonitrile-0.1% formic acid as mobile phase with the flow rate as 0.3 mL•min-1. Injection volume was 10 µL. Positive ionization mode was applied, and the ions were monitored in the multiple reaction monitoring (MRM) mode with curtain gas 0.069 MPa, collision gas 0.052 MPa, ESI ion spray voltage 5000 V, temperature 550 °C, nebulizer gas 0.24 MPa, and turbo gas 0.28 MPa. The limit of detection (LOD) and limit of quantitation (LOQ) of the proposed method are 1 μg•kg-1and 5 μg•kg-1, respectively. The average recoveries of the four pesticides at 10, 20, and 50 µg•kg-1spiking levels range from 77.4% to 95.3%. TheSupersSuperscript textcript textrelative standard deviation (RSD) (n=6) range form 11.83% to 4.52%.

scholarly journals Determination of 77 Multiclass Pesticides and Their Metabolitesin Capsicum and Tomato Using GC-MS/MS and LC-MS/MS

Molecules ◽  
2021 ◽  
Vol 26 (7) ◽  
pp. 1837
Author(s):  
Harischandra Naik Rathod ◽  
Bheemanna Mallappa ◽  
Pallavi Malenahalli Sidramappa ◽  
Chandra Sekhara Reddy Vennapusa ◽  
Pavankumar Kamin ◽  
...  
Keyword(s):  
Limit Of Detection ◽  
Solid Phase ◽  
Graphitized Carbon Black ◽  
Limit Of Quantification ◽  
Gas And Liquid Chromatography ◽  
Relative Standard ◽  
The Matrix ◽  
Liquid Chromatography Tandem Mass ◽  
Primary Secondary Amine

A quick, sensitive, and reproducible analytical method for the determination of 77 multiclass pesticides and their metabolites in Capsicum and tomato by gas and liquid chromatography tandem mass spectrometry was standardized and validated. The limit of detection of 0.19 to 10.91 and limit of quantification of 0.63 to 36.34 µg·kg−1 for Capsicum and 0.10 to 9.55 µg·kg−1 (LOD) and 0.35 to 33.43 µg·kg−1 (LOQ) for tomato. The method involves extraction of sample with acetonitrile, purification by dispersive solid phase extraction using primary secondary amine and graphitized carbon black. The recoveries of all pesticides were in the range of 75 to 110% with a relative standard deviation of less than 20%. Similarly, the method precision was evaluated interms of repeatability (RSDr) and reproducibility (RSDwR) by spiking of mixed pesticides standards at 100 µg·kg−1 recorded anRSD of less than 20%. The matrix effect was acceptable and no significant variation was observed in both the matrices except for few pesticides. The estimated measurement uncertainty found acceptable for all the pesticides. This method found suitable for analysis of vegetable samples drawn from market and farm gates.

scholarly journals Development and Validation of 13-plex Luminex-Based Assay for Measuring Human Serum Antibodies to Streptococcus pneumoniae Capsular Polysaccharides

mSphere ◽  
2018 ◽  
Vol 3 (4) ◽  
pp. e00128-18 ◽  
Author(s):  
Danka Pavliakova ◽  
Peter C. Giardina ◽  
Soraya Moghazeh ◽  
Shite Sebastian ◽  
Maya Koster ◽  
...  
Keyword(s):  
Human Serum ◽  
Lower Limit ◽  
Immunosorbent Assay ◽  
Enzyme Linked Immunosorbent Assay ◽  
Igg Antibodies ◽  
Igg Antibody ◽  
Correlate Of Protection ◽  
Immune Correlate ◽  
Relative Standard ◽  
Limit Of Quantitation

ABSTRACT A Luminex-based direct immunoassay (dLIA) platform has been developed to replace the standardized pneumococcal enzyme-linked immunosorbent assay platform. The multiplex dLIA simultaneously measures the concentration of serum immunoglobulin G (IgG) antibodies specific for pneumococcal capsular polysaccharide (PnPS) serotypes 1, 3, 4, 5, 6A, 6B, 7F, 9V, 14, 18C, 19A, 19F, and 23F. The assay uses poly-l-lysine (PLL)-conjugated PnPS, chemically coupled to spectrally distinct Luminex microspheres. Assay validation experiments were performed using residual human serum samples obtained from 13-valent pneumococcal conjugate vaccine (13vPnC) clinical studies. Assay results are expressed as IgG antibody concentrations in micrograms per milliliter using the international reference serum, 007sp. The lower limit of quantitation (LLOQ) for all serotypes covered in the 13-plex dLIA fell within the range of 0.002 to 0.038 µg/ml serum IgG. The difference between the lower limit and upper limit of the assay range was >500-fold for all serotypes, and assay variability was <20% relative standard deviation (RSD) for all serotypes. IgG antibody measurements were shown to be serotype-specific (some cross-reactivity was observed only between the structurally related serotypes 6A and 6B as well as 19A and 19F), and no interference was observed between the serotypes when the assay was performed in the 13-plex format compared to the singleplex assays. The 13-plex dLIA platform developed by Pfizer Inc. generates up to 143 test results in a single 96-well plate and is a suitable replacement of the enzyme-linked immunosorbent assay (ELISA) platform for evaluating vaccine clinical trials. IMPORTANCE The pneumococcal enzyme-linked immunosorbent assay (ELISA) measures IgG antibodies in human serum, and it is an important assay that supports licensure of pneumococcal vaccines. The immune correlate of protection, 0.35 µg/ml of IgG antibodies, was determined by the ELISA method. Pfizer has developed a new Luminex-based assay platform to replace the ELISA. These papers describe the important work of (i) validating the Luminex-based assay and (ii) bridging the immune correlate of protection (0.35 µg/ml IgG) to equivalent values reported by the Luminex platform.

scholarly journals Development of a method for the measurement of dehydroepiandrosterone sulphate by liquid chromatography-tandem mass spectrometry

2005 ◽  
Vol 42 (6) ◽  
pp. 468-474 ◽  
Author(s):  
C A Chadwick ◽  
L J Owen ◽  
B G Keevil
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Lower Limit ◽  
Internal Standard ◽  
Tandem Mass ◽  
Dehydroepiandrosterone Sulphate ◽  
Chromatography Tandem Mass Spectrometry ◽  
Limit Of Quantitation ◽  
Liquid Chromatography Tandem Mass

Background: Dehydroepiandrosterone sulphate (DHEAS) is a steroid that is increasingly being recognized as a potential drug of abuse in many countries. This is due to its reputation as a hormone that may be able to retard the ageing process. The measurement of DHEAS is useful in the diagnosis of medical conditions such as congenital adrenal hyperplasia and polycystic ovary syndrome. Thus, a liquid chromatography-tandem mass spectrometry method has been developed to determine DHEAS concentrations in human serum. Method: The chromatography was performed using a WatersTM 2795 Alliance HT LC system coupled to a Mercury Fusion-RP column fitted with a SecurityGuardTM column. Results: DHEAS and the internal standard, deuterated DHEAS, both had a retention time of 1.5 min. The transition determined by the Micromass QuattroTM tandem mass spectrometer for DHEAS was m/z 367.3>96.7 and for the internal standard m/z 369.3>96.6. The method was linear up to 20 µmol/L; the lower limit of detection and the lower limit of quantitation were both 1 µmol/L. The intra- and interassay imprecision were <11% over a concentration range of 1-18 µmol/L for the in-house quality control and <12% for the intra- and interassay imprecision for the Bio-Rad Lyphocheck QC. Conclusion: The measurement of DHEAS by liquid chromatography-tandem mass spectrometry is robust and has a simple sample preparation procedure with a rapid cycle time of only 4 min.

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