Simultaneous determination of anthraquinone derivatives in Radix et Rhizoma Rhei-based medicines by ultra-performance LC-ESCI-MS/MS multiple reaction monitoring

2014 ◽  
Vol 26 (2) ◽  
pp. 229-242 ◽  
Author(s):  
G.-Y. Wang ◽  
Y.-P. Shi
2018 ◽  
Vol 2018 ◽  
pp. 1-12 ◽  
Author(s):  
Huizi Ouyang ◽  
Fang Liu ◽  
Zhidan Tang ◽  
Xiaopeng Chen ◽  
Fang Bo ◽  
...  

A sensitive and reliable LC-MS/MS method has been developed and validated for simultaneous determination of six Aconitum alkaloids (aconitine, hypaconitine, mesaconitine, benzoylaconitine, benzoylhypacoitine, and benzoylmesaconine) and seven ginsenosides (Rb1, Rb2, Rc, Rd, Re, Rf, and Rg1) in rat plasma after oral administration of Shen-Fu prescription. Psoralen was selected as internal standard (IS). Protein precipitation with methanol was used in sample preparation. The chromatographic separation was achieved on a CORTECS™ C18 column with 0.1% formic acid aqueous solution and acetonitrile as mobile phase. The flow rate was 0.3 mL/min. The detection was performed on a tandem mass system with an electrospray ionization (ESI) source in the positive ionization and multiple-reaction monitoring (MRM) mode. The calibration curves of six Aconitum alkaloids and seven ginsenosides were linear over the range of 0.1-50 and 1-500 ng/mL, respectively. The extraction recoveries of the analytes in plasma samples ranged from 64.2 to 94.1%. Meanwhile, the intra- and interday precision of the analytes were less than 14.3%, and the accuracy was in the range of −14.2% to 9.8%. The developed method was successfully applied to the pharmacokinetics of six Aconitum alkaloids and seven ginsenosides in rat plasma after oral administration of Shen-Fu prescription.


RSC Advances ◽  
2016 ◽  
Vol 6 (75) ◽  
pp. 70990-70998 ◽  
Author(s):  
Qikun Jiang ◽  
Yan Liu ◽  
Yunjie Wang ◽  
Yinghua Sun ◽  
Bo Li ◽  
...  

The study's aim is to develop and validate a rapid, selective and sensitive ultra-performance liquid chromatography-tandem mass spectrometry with multiple reaction monitoring (MRM) mode method for the simultaneous determination of entecavir and lamivudine in rat plasma.


2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.


2013 ◽  
Vol 634-638 ◽  
pp. 1586-1590
Author(s):  
Su Fang Wang ◽  
Shou Jie Zhang ◽  
Chun Hong Dong ◽  
Guo Qing Wang ◽  
Jun Feng Guo ◽  
...  

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%.


2020 ◽  
Vol 32 (2) ◽  
pp. 145-148 ◽  
Author(s):  
Siyuan Chen ◽  
Jianshe Ma ◽  
Xianqin Wang ◽  
Peiwu Geng

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.


2017 ◽  
Vol 33 (7) ◽  
pp. 863-867 ◽  
Author(s):  
Maya KAMAO ◽  
Yoshihisa HIROTA ◽  
Yoshitomo SUHARA ◽  
Naoko TSUGAWA ◽  
Kimie NAKAGAWA ◽  
...  

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