scholarly journals Multiple-Reaction Monitoring Tandem Mass Method for Determination of Phenolics and Water-Soluble Vitamins in Eccoilopus formosanus

Molecules ◽  
2020 ◽  
Vol 25 (16) ◽  
pp. 3632
Author(s):  
Ho-Shin Huang ◽  
Hsu-Sheng Yu ◽  
Chia-Hung Yen ◽  
Ean-Tun Liaw
Keyword(s):  
Multiple Reaction Monitoring ◽  
Correlation Coefficients ◽  
Ion Source ◽  
Water Soluble ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Cereal Grain ◽  
Relative Standard ◽  
Qualitative Determination

This study established a validated method for the quantitative and qualitative determination of eight signature compounds in Eccoilopus formosanus. We used multiple-reaction monitoring scanning for quantification, and switched the electrospray ion source polarity between positive and negative modes in a single chromatographic run. The precursor-to-product ion transitions were m/z 355/163, m/z 181/163, m/z 265/122, m/z 269/117, m/z 170/152, m/z 377.2/180.7, m/z 169/124.8 and m/z 193/134 for chlorogenic acid, caffeic acid, thiamine, apigenin, pyridoxamin, riboflavin, gallic acid and ferulic acid, respectively. The developed method was also validated for accuracy, precision and limit of quantification. In this method, eight compounds were quantified with correlation coefficients of greater than 0.995. A high recovery (81.5–94.1%) and good reproducibility was obtained for five phenolics and three vitamins with the relative standard deviation, ranging from 1.2 to 3.5%. This method may be applied to the determination of both phenolics and water-soluble vitamins in cereal grain. The results may suggest that the extract of E. formosanus could be a good source of bioactive phytochemicals.

scholarly journals Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

2015 ◽  
Vol 12 (1) ◽  
pp. 167-177 ◽  
Author(s):  
Baghdad Science Journal
Keyword(s):  
Limit Of Detection ◽  
Pharmaceutical Preparations ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Forms ◽  
Salbutamol Sulphate ◽  
Phenylephrine Hydrochloride ◽  
Relative Standard ◽  
Metoclopramide Hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision.

scholarly journals UPLC–MS/MS simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, MDMA, and MDA in hair

2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng
Keyword(s):  
Simultaneous Determination ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Ammonium Hydroxide ◽  
Ultra Performance Liquid Chromatography ◽  
Acetate Solution ◽  
Hair Samples ◽  
Relative Standard

Hair is a stable specimen and has a longer detection window (from weeks to months) than blood and urine. Through the analysis of hair, the long-term information of the drug use of the identified person could be explored. Our work is to establish an ultra-performance liquid chromatography–tandem mass spectroscopy (UPLC–MS/MS) method for simultaneous determination of methamphetamine, amphetamine, morphine, monoacetylmorphine, ketamine, norketamine, 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyamphetamine (MDA) in hair. Methoxyphenamine was used as an internal standard. The chromatographic separation was performed on a UPLC ethylene bridged hybrid (BEH) C18 (2.1 mm × 50 mm, 1.7 μm) column using a mobile phase of acetonitrile–water with 10 mmol/L ammonium acetate solution which containing 0.05% ammonium hydroxide. The multiple reaction monitoring in positive electrospray ionization was used for quantitative determination. The intra-day and inter-day precisions (relative standard deviation [RSD]) were below 15%. The accuracy ranged between 85.5% and 110.4%, the average recovery rate was above 72.9%, and the matrix effect ranged between 92.7% and 109.2%. Standard curves were in the range of 0.05–5.0 ng/mg, and the correlation coefficients were greater than 0.995. The established UPLC–MS/MS method was applied to analyze the hair samples successfully.

scholarly journals Simultaneous Determination of Ropivacaine and 3-Hydroxy Ropivacaine in Cerebrospinal Fluid by UPLC-MS/MS

2020 ◽  
Vol 2020 ◽  
pp. 1-6
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Quan Zhou
Keyword(s):  
Cerebrospinal Fluid ◽  
Extraction Efficiency ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Liquid Liquid Extraction ◽  
The Matrix ◽  
Interday Precision

In this paper, a UPLC-MS/MS method was developed for the determination of ropivacaine and its metabolite 3-hydroxy ropivacaine in cerebrospinal fluid. The cerebrospinal fluid was processed by ethyl acetate liquid-liquid extraction. The multiple reaction monitoring (MRM) mode was used for quantitative analysis by monitoring the transitions of m/z 275.3 → 126.2 for ropivacaine, m/z 291.0 → 126.0 for 3-hydroxy ropivacaine, and m/z 290.2 → 198.2 for the internal standard. Standard curves for ropivacaine and 3-hydroxy ropivacaine in cerebrospinal fluid were conducted over the concentration range of 0.2–2000 ng/mL, demonstrating excellent linearity, and the lower limit of quantification was 0.2 ng/mL. The intraday precision of ropivacaine and 3-hydroxy ropivacaine was less than 11%, while the interday precision was less than 7%. The accuracy ranged between 87% and 107%, the average extraction efficiency was higher than 79%, and the matrix effect was between 89% and 98%. The developed method was then applied to a case of suspected poisoning of ropivacaine.

scholarly journals Determination of 5-nitro-2-furaldehyde as marker residue for nitrofurazone treatment in farmed shrimps and with addressing the use of a novel internal standard

2019 ◽  
Vol 9 (1) ◽  
Author(s):  
Qiang Wang ◽  
Xu-Feng Wang ◽  
Yong-Yuan Jiang ◽  
Zhi-Guang Li ◽  
Nan Cai ◽  
...  
Keyword(s):  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass ◽  
Negative Ionization ◽  
Ultrasonic Manipulation

AbstractWe developed a significantly improved ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of 5-nitro-2-furaldehyde (NF) as a surrogate using a novel internal standard for the detection of nitrofurazone. We used 2,4-dinitrophenylhydrazine derivatization and furfural as the internal standard. Derivatization was easily performed in HCl using ultrasonic manipulation for 5 min followed by liquid extraction using ethyl acetate. The samples were concentrated and purified using reverse phase and alumina cartridges in tandem. The derivatives were separated using a linear gradient elution on a C18 column with methanol and water as the mobile phase in negative ionization mode and multiple reaction monitoring. Under the optimized conditions, the calibration curves were linear from 0.2 to 20 μg/L with correlation coefficients >0.999. Mean recoveries were 80.8 to 104.4% with the intra- and inter-day relative standard deviations <15% at spiking levels of 0.1 to 10 μg/kg. The limits of detection and quantification were 0.05 and 0.1 μg/kg, respectively. This method is a robust tool for the identification and quantitative determination of NF in shrimp samples.

scholarly journals Determination of Niacin in Food Materials by Liquid Chromatography Using Isotope Dilution Mass Spectrometry

2007 ◽  
Vol 90 (4) ◽  
pp. 1084-1089 ◽  
Author(s):  
Robert J Goldschmidt ◽  
Wayne R Wolf
Keyword(s):  
Liquid Chromatography ◽  
Reference Materials ◽  
Isotope Dilution ◽  
Solid Phase ◽  
Multiple Reaction Monitoring ◽  
Isotope Dilution Mass Spectrometry ◽  
Water Soluble ◽  
Relative Standard ◽  
Interference Problems

Abstract The availability of deuterium-labeled nicotinic acid makes stable isotope dilution mass spectromerty (MS) coupled with liquid chromatography (LC) an attractive option for the determination of the water-soluble B-vitamin niacin in food samples. A method was developed based on acid digestion, solid-phase extraction with a strong cation exchange column, and reversed-phase chromatography with a C18 column. Detection is by positive ion electrospray MS. Analysis in selected ion recording mode is subject to interference problems similar to those found with other LC determinations of niacin, but the additional selectivity of multiple reaction monitoring mode largely eliminates interference problems. The method was applied to 6 different food matrixes and to appropriate reference materials, including milk samples with niacin levels near 1 ppm. The method exhibited good accuracy, based on levels obtained for the reference materials, and relative standard deviations in the range of 0.55%.

scholarly journals Determination of Methylene Blue and Its Metabolite Residues in Aquatic Products by High-Performance Liquid Chromatography–Tandem Mass Spectrometry

Molecules ◽  
2021 ◽  
Vol 26 (16) ◽  
pp. 4975
Author(s):  
Xuan Zhang ◽  
Yunhua Hui ◽  
Changling Fang ◽  
Yuan Wang ◽  
Feng Han ◽  
...  
Keyword(s):  
Methylene Blue ◽  
High Performance ◽  
Correlation Coefficients ◽  
Limit Of Quantification ◽  
Aquatic Products ◽  
Azure B ◽  
Chromatography Tandem Mass Spectrometry ◽  
Relative Standard ◽  
Liquid Chromatography Tandem Mass

A sensitive and reliable method was developed to determine methylene blue (MB) and its metabolite residues, including azure A (AZA), azure B (AZB), and azure C (AZC) in aquatic products by HPLC–MS/MS. The samples were extracted by acetonitrile and cleaned up by alumina-neutral (ALN) cartridges. The analytes were separated on a Sunfire C18 column (150 mm × 2.1 mm, 5 µm). The method was validated according to the European criteria of Commission Decision 2002/657/CE. Good linearity between 1–500 µg/L was obtained with correlation coefficients (R2) greater than 0.99. The limit of quantification (LOQ) was 1.0 µg/kg. The average recoveries at three levels of each compound (1, 5, and 10 µg/kg) were demonstrated to be in the range of 71.8–97.5%, with relative standard deviations (RSDs) from 1.05% to 8.63%. This method was suitable for the detection of methylene blue and its metabolite residues in aquatic products.

scholarly journals Simultaneous Determination of Three Bioactive Constituents from Bletilla striata by UPLC-MS/MS and Application of the Technique to Pharmacokinetic Analyses

2019 ◽  
Vol 2019 ◽  
pp. 1-10
Author(s):  
Hao Chen ◽  
Lin Zheng ◽  
Chao-Ye Mei ◽  
Zi-Peng Gong ◽  
Yong-Jun Li ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Enterohepatic Circulation ◽  
Multiple Reaction Monitoring ◽  
Active Ingredients ◽  
Bioactive Constituents ◽  
Limit Of Quantification ◽  
Time Curve ◽  
Bletilla Striata ◽  
Relative Standard

Bletilla striata has been widely used as a valuable hemostatic agent for thousands of years due to the high levels of bioactive constituents it contains. Here, we used a sensitive ultrahigh-performance liquid chromatography-tandem mass spectroscopy (UPLC-MS/MS) method for the simultaneous determination of three major active ingredients of the B. striata extract, namely, α-isobutylmalic acid, gymnoside I, and militarine in rat plasma. The three major active ingredients were determined using the multiple reaction monitoring (MRM) mode at m/z 189 ⟶ 129 for α-isobutylmalic acid, m/z 457.2 ⟶ 285.1 for gymnoside I, m/z 725.3 ⟶ 457.2 for militarine, and m/z 417.0 ⟶ 267.0 for the IS puerarin. All calibration curves showed good linearity (R2 ≥ 0.999) over the concentration range with the lower limit of quantification between 0.015 and 0.029 μg/mL. The relative standard deviations of intraday and interday measurements were less than 15%, and the method was accurate within 93.3–100.4%. The extraction recovery was 92.65–100.98%, and no matrix effect was observed. The results indicated that after oral administration of B. striata in rats, the Tmax of α-isobutylmalic acid was significantly longer than that of gymnoside I and militarine and the mean residence time and area under the curve of α-isobutylmalic acid and gymnoside I in rats were significantly higher than those of militarine. Moreover, the blood concentration-time curve of α-isobutylmalic acid showed double peaks, suggesting that α-isobutylmalic acid could exhibit the phenomenon of enterohepatic circulation or metabolic conversion. We also explored some of the pharmacokinetic characteristics of three ingredients from B. striata extract in vivo, and the data obtained may provide a basis for the further investigation of B. striata.

scholarly journals Enantioseparation and Determination of Penconazole in Rat Plasma by Chiral LC-MS/MS: Application to a Stereoselective Toxicokinetic Study

Molecules ◽  
2020 ◽  
Vol 25 (13) ◽  
pp. 2964
Author(s):  
Siman Ma ◽  
Jia Lun ◽  
Yanru Liu ◽  
Zhen Jiang ◽  
Xingjie Guo
Keyword(s):  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Correlation Coefficients ◽  
Rat Plasma ◽  
Male Rats ◽  
Ionization Source ◽  
Established Method ◽  
Relative Standard

In this study, a specific and sensitive method of liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed for the determination of penconazole enantiomers in rat plasma. The enantioseparation was achieved on a Chiralpak IC column by using acetonitrile/water (80:20, v/v) as the mobile phase. Penconazole enantiomers and internal standard l-lansoprazole (IS) were detected in multiple reaction monitoring (MRM) mode with positive electrospray ionization source. The method was validated over the concentration range of 2.5–250.0 ng mL−1 for penconazole enantiomers. Good linearity was obtained for both enantiomers with correlation coefficients (R) greater than 0.995. The relative error was well within the admissible range of −1.1–3.2%, and relative standard deviation was less than 6.0%. After validation, the established method was successfully applied to a stereoselective toxicokinetic study in female and male rats after oral administration of 50 mg kg−1 racemic penconazole. This is the first experiment regarding the stereospecific toxicokinetic study of penconazole and the bioanalytical approach for its quantitation in vivo.

scholarly journals Fingerprint and multi-component quantitative analyses for quality evaluation of Rhizoma coptidis steamed with rice wine

2021 ◽  
Vol 18 (6) ◽  
pp. 1297-1303
Author(s):  
Jin Wang ◽  
Hai-rong Zeng ◽  
Guan-hua Lou ◽  
Chang-jiang Hu ◽  
Qin-wan Huang ◽  
...  
Keyword(s):  
High Performance ◽  
Quality Evaluation ◽  
Multiple Reaction Monitoring ◽  
Reaction Monitoring ◽  
Rice Wine ◽  
Rhizoma Coptidis ◽  
Relative Standard ◽  
Multiple Reaction Monitoring Mode ◽  
Quantitative Analyses

Purpose: To establish a method for the simultaneous determination of multi-components of Rhizoma coptidis steamed with rice wine (RCRW), and to provide a reference for assessing its standard of quality. Method: Chromatographic separation was performed on a high performance liquid chromatography (HPLC) system to determine the characteristic fingerprint of RCRW. The mobile phase consisted of acetonitrile (A) and 0.1 % trifluoroacetic acid (B), with gradients of B as follows: 15 - 20 % from 0 – 30 min; 20 - 25 % from 30 - 50 min; 25 - 35 % for 50 - 60 min, and 35 % for 60 - 70 min. Results: In the multiple reaction monitoring mode, eight components of RCRW were isolated by HPLCphoto-diode array (PDA) method. A fingerprint of the RCRW was established and 8 peaks were calibrated. The method was further validated in terms of linearity (R2 > 0.9993), precision (relative standard deviation, RSD < 1.51 %); repeatability (RSD < 2.98 %) and stability (RSD < 1.93 %). Mean recovery rate ranged from 96.2 to 103.8 %, while RSD values ranged from 0.92 to 2.88 %. Conclusion: These results show that HPLC-PDA method is accurate and feasible, and that they provide a reference for further comprehensive and effective quality control of RCRW.

Determination of Shanzhiside Methylester in Rat Plasma by Uplc-Ms/Ms and its Application to a Pharmacokinetic Study

2020 ◽  
Vol 16 (7) ◽  
pp. 960-966
Author(s):  
Qinghua Weng ◽  
Yichuan Chen ◽  
Zuoquan Zhong ◽  
Qianqian Wang ◽  
Lianguo Chen ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Multiple Reaction Monitoring ◽  
Internal Standard ◽  
Gradient Elution ◽  
Rat Plasma ◽  
Precipitation Method ◽  
Reaction Monitoring ◽  
Limit Of Quantification ◽  
Pharmacokinetics In Rats

Introduction: In this study, we used UPLC-MS/MS to detect shanzhiside methylester in rat plasma, and investigated its pharmacokinetics in rats. Materials and Methods: Diazepam was utilized as an internal standard (IS), and acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC BEH C18 column using mobile phase of methanol-0.1 % formic acid with gradient elution. Electrospray ionization (ESI) tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied. Results: The results indicated that within the range of 5-4000 ng/mL, linearity of shanzhiside methylester in rat plasma was acceptable (r>0.995), and the lower limit of quantification (LLOQ) was 5 ng/mL. Intra-day and inter-day precision RSD of shanzhiside methylester in rat plasma were lower than 14%. Accuracy range was between 87.3 % and 109.1 %, and matrix effect was between 99.2% and 106.3%. Conclusion: The method was successfully applied in the pharmacokinetics of shanzhiside methylester in rats after intravenous administration.

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