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

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.

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

Advanced Materials Research ◽

10.4028/www.scientific.net/amr.634-638.1586 ◽

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%.

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Simultaneous Determination of Eight New Generation Amide Insecticide Residues in Complex Matrix Agri-food by Multi-walled Carbon Nanotube Cleanup and UPLC-MS/MS

10.21203/rs.3.rs-952153/v1 ◽

2021 ◽

Author(s):

Tao Lin ◽

Xinglian Chen ◽

Li Wang ◽

Haixian Fang ◽

Maoxuan Li ◽

...

Keyword(s):

Mass Spectrometry ◽

Simultaneous Determination ◽

High Performance ◽

Rapid Determination ◽

Complex Matrix ◽

Limit Of Quantification ◽

Relative Standard ◽

The Matrix ◽

Multi Walled Carbon Nanotubes

Abstract The simultaneous determination method of 8 amide pesticides by multi-walled carbon nanotubes (MWCNs) cleanup, combined with QuEChERS method and ultra-high performance liquid chromatography-triple quadrupole tandem mass spectrometry has been developed and successfully applied in complex matrix such as green onions, celery, leeks, citrus, lychees, avocado. The matric effect of MWCNs is optimized and compared with QuEChERS materials. The results show that MWCNs can effectively reduce the matrix effect in sample extraction. The mass spectrometry is optimized, through their chemical structure skeletons, the ESI+ and ESI- mode are simultaneously scanned in the method. The coefficient (r) is greater than 0.9990, the limit of quantification ranges from 0.03 to 0.80 μg/kg, the recovery rate ranges from 71.2% to 120%, and the relative standard deviation (RSD) ranges from 3.8% to 9.4%. The method is fast, simple, sensitive, and has good purification effect. It is suitable for the rapid determination of amide pesticides in complex matrix agri-food.

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

Acta Chromatographica ◽

10.1556/1326.2019.00615 ◽

2020 ◽

Vol 32 (2) ◽

pp. 145-148 ◽

Cited By ~ 1

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.

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Simultaneous determination of five pesticides residues in Anoectochilus roxburghii by HPLC-MS/MS method

Pharmaceutical Care and Research ◽

10.5428/pcar20200506 ◽

2020 ◽

Vol 20 (5) ◽

pp. 345-349

Author(s):

Liqun WU ◽

◽

Mingke LUO ◽

Wensheng HE ◽

Wenting CHEN

Keyword(s):

Simultaneous Determination ◽

Multiple Reaction Monitoring ◽

Gradient Elution ◽

Acetonitrile Solution ◽

Ionization Source ◽

Thiophanate Methyl ◽

Pesticides Residues ◽

Relative Standard ◽

Anoectochilus Roxburghii

Objective： To establish a HPLC-MS/MS method for simultaneous determination of five pesticides residues including tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin in Anoectochilus roxburghii.Methods： The samples were extracted by acetonitrile solution and purified by QuEChERS method.Separation was performed on Agilent Eclipse Plus C18 column（50 mm×2.1 mm，1.8 μm） with the mobile phase consisting of 0.1% formic acid（A） and acetonitrile（B） by gradient elution（0-1.0 min，90% A；1.0-3.0 min，90%-70% A;3.0-5.0 min，70%-30% A;5.0-8.0 min，30%-10% A;8.0-14.0 min，10% A;14.0-15.0 min，10%-90% A;15.0-17.0 min，90% A）.Detection was performed on a triple quadrupole tandem mass spectrometry with electrospray ionization source operating in positive ion mode under multiple reaction monitoring（MRM） mode.Results： The calibration curves of five pesticides showed good linearity coefficients（r>0.99）.The average recoveries ranged from 72.7% to 94.9%（n=6），and the relative standard derivations（RSDs） were within 1.8%-10.3%（n=6）.The detection limits of tebuconazole，metalaxyl-M，thiophanate-methyl，oxytetracycline and abamectin were 0.6，0.2，0.3，0.2，5.0 μg/kg，and the quantitation limits of 5 pesticides were 2.0，0.5，1.0，0.6 and 10.0 μg/kg respectively.Conclusion： The established method was proved to be sensitive，simple and reliable，and could be applied for the determination of these five pesticides in Anoectochilus roxburghii and quality control in the planting process.

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Simultaneous Determination of 12 Bioactive Constituents in Bupi Yiqi No. 1 Recipe by Ultrahigh-Performance Liquid Chromatography Tandem Mass Spectrometry

Journal of AOAC International ◽

10.5740/jaoacint.19-0162 ◽

2020 ◽

Vol 103 (1) ◽

pp. 117-123

Author(s):

Qingling Xie ◽

Bin Li ◽

Feibing Huang ◽

Mengru Cao ◽

Hanwen Yuan ◽

...

Keyword(s):

Simultaneous Determination ◽

Multiple Reaction Monitoring ◽

Cancer Recurrence ◽

Correlation Coefficients ◽

Bioactive Constituents ◽

Column Temperature ◽

Ginsenoside Re ◽

Esi Ms ◽

Stability And Accuracy

Abstract Background: Bupi Yiqi No. 1 Recipe (BPYQ), a traditional Chinese medicine formula, has been widely used as a treatment of multidrug resistance during chemotherapy in colorectal cancer and for the prevention of gastrointestinal cancer recurrence for decades. Objective: In this study, a rapid, reliable, and accurate ultrahigh-performance LC (UHPLC) coupled with electrospray ionization (ESI)–tandem MS (MS/MS) method was developed for the simultaneous determination of 12 major bioactive components, including protocatechuic acid, astilbin, rutin, calycosin-7-O-β-D-glucoside, ginsenoside Re, ononin, isoliquiritigenin, calycosin, apigenin, ginsenoside Rb1, formononetin, and glycyrrhizic acid in BPYQ. Methods: The chromatographic separation of the analytes was achieved on a Poroshell 120 SB-Aq column (50 × 2.1 mm, 1.7 µm) with a mobile phase of acetonitrile and 0.1% (v/v) formic acid aqueous solution. The flow rate and column temperature were set at 0.4 mL/min and 30°C, respectively. Mass spectrometric detection of the analyses was performed on multiple reaction monitoring mode in positive and negative ESI mode. Results: The established UHPLC–ESI–MS/MS method was validated in terms of the linearity, precision, repeatability, stability, and accuracy. All calibration curves of the 12 compounds showed good linearity, with correlation coefficients (r) greater than 0.9980 within the test ranges. The LODs and LOQs for the 12 compounds were in the ranges of 0.08–1.32 and 0.27–5.28 ng/mL, respectively. The average recoveries of all the standard compounds were between 98.4 and 102.9%, and their relative SD values ranged from 1.24 to 3.78%. Conclusions: The proposed method can provide a meaningful basis for the QC of BPYQ. Highlights: The established UHPLC-ESI-MS/MS method was demonstrated to be a powerful tool for quantifying the 12 compounds in BPYQ.

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Simultaneous Determination of Phenolic Acids, Anthraquinones, and Flavonoids in the Aerial Part and the Fruit of Xanthium Sibiricum by LC- ESI- QTRAP-MS/MS

Current Pharmaceutical Analysis ◽

10.2174/1573412914666180502125549 ◽

2019 ◽

Vol 15 (5) ◽

pp. 542-553

Author(s):

Hui Zhao ◽

Hao Cai ◽

Juan-Xiu Liu ◽

Sheng-Nan Wang ◽

Xun-Hong Liu ◽

...

Keyword(s):

Simultaneous Determination ◽

Phenolic Acids ◽

High Performance ◽

Aerial Part ◽

Multiple Reaction Monitoring ◽

Principal Component ◽

Negative Ion ◽

Xanthium Sibiricum ◽

Relative Standard

Background: Xanthium sibiricum is a well-known traditional Chinese medicine (TCM) that has been commonly used to treat rhinitis and related nasal diseases. The aim of this study was to develop a comprehensive analytical method based on high-performance liquid chromatographyelectrospray ionization coupled with triple quadrupole-linear ion trap mass spectrometry (LC-ESIQTRAP- MS/MS) for the simultaneous determination of phenolic acids, anthraquinones, and flavonoids in the aerial part and fruit of Xanthium sibiricum. Methods: The separation was completed on Agilent ZORBAX SB-C18 column (250 × 4.6 mm, 5μm) using methanol and 0.2% (v/v) aqueous formic acid as the mobile phase. The target components were analyzed in negative ion mode with accurate and sensitive multiple reaction monitoring (MRM) mode. Results: The correlation coefficients of all the calibration curves were higher than 0.9994. Relative standard deviations of intra- and inter-day precisions of the eighteen components were all lower than 2.87% and the recoveries were in the range from 97.73% to 101.82%. The validated method was successfully applied to possess forty Xanthium sibiricum samples (Xanthii Herba, Xanthii Fructus, and processed Xanthii Fructus) collected from different places in P. R. China. Furthermore, principal component analysis (PCA) was performed to evaluate and classify the samples according to the contents of the eighteen bioactive components. Conclusion: All the results demonstrated that the developed method was useful and could be applied for the overall assessment of the quality of Xanthii Herba and Xanthii Fructus.

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Simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace by UHPLC-MS/MS

World Mycotoxin Journal ◽

10.3920/wmj2013.1565 ◽

2014 ◽

Vol 7 (2) ◽

pp. 121-129 ◽

Cited By ~ 5

Author(s):

L. Luan ◽

N. Chen ◽

Z. Han ◽

X. Liu ◽

Y. Zheng ◽

...

Keyword(s):

Simultaneous Determination ◽

Mycophenolic Acid ◽

Solid Phase ◽

Multiple Reaction Monitoring ◽

Reversed Phase ◽

Grape Pomace ◽

Relative Standard ◽

Ultrahigh Performance Liquid Chromatography ◽

Aflatoxin B

A reliable ultrahigh performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of aflatoxin B1, aflatoxin B2, mycophenolic acid and sterigmatocystin in grape pomace. The samples were extracted by acetonitrile aqueous solution and further purified using a solid-phase extraction-based homemade clean-up cartridge. Next, the analytes were separated on a reversed-phase C18 column with a mobile phase consisting of water and acetonitrile. The separated compounds were detected with a tandem quadrupole mass spectrometer operating in positive electro-spray ionisation mode using multiple reaction monitoring. The established method was extensively validated by determining linearity (R2≯0.999), recovery (97.5-102.8%) and precision (relative standard deviation ≤7.0%). This method was then used for the simultaneous determination of the four mycotoxins in grape pomace samples.

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

Molecules ◽

10.3390/molecules25163632 ◽

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.

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Simultaneous Determination of Aspirin and Rosuvastatin Calcium in Capsules by Using RP-HPLC Coupled with Photo Diode Array Detection

International Letters of Chemistry Physics and Astronomy ◽

10.18052/www.scipress.com/ilcpa.33.218 ◽

2014 ◽

Vol 33 ◽

pp. 218-230

Author(s):

Ankita Panchal ◽

Gaurav Sanghvi ◽

Ashish Vachhani ◽

Navin Sheth ◽

Devendra Vaishnav

Keyword(s):

Quality Control ◽

Simultaneous Determination ◽

Lower Limit ◽

Limit Of Detection ◽

Pharmaceutical Formulations ◽

Coefficient Of Determination ◽

Limit Of Quantification ◽

Relative Standard ◽

Rosuvastatin Calcium

A simple, sensitive, specific, and cost effective method for simultaneous determination of Aspirin and Rosuvastatin calcium was developed and validated in single dosage formulation. The sample solution of ASP and RSTC was prepared using methanol as a solvent. Separation of ASP and RSTC was achieved with a mobile phase consisting of 20 mM KH2PO4 : Methanol (30:70 v/v) at a flow rate of 1.0 ml/min. Separations were performed on Merck hibar 250-4.6 RP18 (5 µm) column (150 mm X 3.0 mm), using a Shimadzu Prominence HPLC system equipped with a Shimadzu SPD-20A detector, Rhenodyne 7725i injector with 20 μL loop, LC-20 AD pump, CBM-20 Alite controller and LC Solution software. Retention times of ASP and RSTC were 3.747 and 5.969 minutes respectively. Absolute recovery of ASP and RSTC was 100.3 and 100.03 % respectively. The lower limit of quantification (LLOQ) of ASP and RSTC was 0.3097 and 0.1063 ppm and lower limit of detection (LLOD) of ASP and RSTC was 0.01535 and 0.01358 ppm respectively. Linearity was established for the range of concentrations 15.00-90.0 μg/ml and 2.0-12.0 μg/ml for ASP and RSTC respectively with the coefficient of determination (R2) of 0.994 and 0.999 for both the compounds. The inter- and intra-day precision in the measurement of ASP quality control (QC) sample 75 μg/ml, were in the range 0.1-0.2 % relative standard deviation (R.S.D.) and 0.2-0.3 % R.S.D., respectively. The inter- and intra-day precision in the measurement of RST quality control (QC) sample 10 μg/ml, were in the range 0.1-0.2 % R.S.D., and 0.0-0.3 % R.S.D., respectively. The developed method would be applicable for routine quality control of ASP And RSTC in bulk as well as in pharmaceutical formulations

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The RP-HPLC method development and validation for simultaneous determination of oryzalin and ethofumesate pesticides in soil and water

Acta Chromatographica ◽

10.1556/1326.2021.00953 ◽

2021 ◽

Author(s):

Shishir Tandon ◽

Suman Lata Pal

Keyword(s):

Simultaneous Determination ◽

Method Development ◽

Hplc Method ◽

Limit Of Quantification ◽

Rp Hplc ◽

Relative Standard ◽

High Throughput Detection ◽

Hplc Method Development ◽

Soil And Water

Abstract A sensitive and reliable method for simultaneous determination of oryzalin and ethofumesate residues in pantnagar soil and water was validated. The compounds were extracted by LLE with dichloromethane from water, and acetone:methanol mixture from soil followed by SPE cleanup. Detection and quantification was done by RP-HPLC using mobile phase methanol:water (70:30, v/v) at 280 nm. The developed method showed satisfactory validation results with linearity (0.99), relative standard deviations (1.55 and 1.73%), and limit of quantification (0.002 μg g−1 and 0.005 μg g−1) for ethofumesate and oryzalin, respectively. Recoveries ranged for oryzalin and ethofumesate from 79.80–90.52, 75.58–86.04% (soil) and 83.50–95.92, 82.28–94.60% (water), respectively. The method could be used for routine high-throughput detection and determination of these compounds.

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