scholarly journals Rapid simultaneous identification and determination of the multiple compounds in crudeFructus Corniand its processed products by HPLC–MS/MS with multiple reaction monitoring mode

2012 ◽  
Vol 51 (3) ◽  
pp. 273-278 ◽  
Author(s):  
Hao Cai ◽  
Gang Cao ◽  
Baochang Cai
2010 ◽  
Vol 93 (5) ◽  
pp. 1666-1671 ◽  
Author(s):  
Xi Xia ◽  
Xiaowei Li ◽  
Shuangyang Ding ◽  
Jianzhong Shen

Abstract A sensitive and reliable method has been developed and validated for the determination of chloramphenicol in poultry and swine liver using SPE and ultra-performance liquid chromatography (UPLC)/MS/MS. The liver samples were extracted with ethyl acetate, defatted with n-hexane, and further cleaned up using SPE cartridges with polymeric sorbent. An Acquity BEH C18 column was used for gradient UPLC separation, with water and acetonitrile as the mobile phase. The multiple reaction monitoring mode was used for two precursor-product ion transitions for chloramphenicol and one for the internal standard. The method was validated at 0.1, 0.3, and 1.0 µg/kg. Mean recoveries from fortified samples ranged from 95.5 to 106.7% with an RSD of 12.2%. The method LOD was <0.02 µg/kg.


2021 ◽  
Vol 18 (6) ◽  
pp. 1297-1303
Author(s):  
Jin Wang ◽  
Hai-rong Zeng ◽  
Guan-hua Lou ◽  
Chang-jiang Hu ◽  
Qin-wan Huang ◽  
...  

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.


2015 ◽  
Vol 98 (3) ◽  
pp. 839-846 ◽  
Author(s):  
Ruoxin Wu ◽  
Qiyong Chen ◽  
Shujing Li ◽  
Guoliang Fan

Abstract A novel, simple, and rapid method for the quantification of 27 commonly used pesticides in ginseng incorporating a modified QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) procedure was developed and validated. The pesticides were extracted with 1% acetic acid in acetonitrile and extracts purified by use of the mixed sorbents primary-secondary amine, C18, and graphitized carbon black. Quantitative analysis of all pesticides was performed by ultra-performance LC/MS/MS in the positive ionization mode in a single run due to the fast polarity switching capability of the mass spectrometer. Two precursor-product ion transitions were monitored for each compound in the multiple reaction monitoring mode. Quantification was carried out using matrix-matched standards for calibration. Recoveries of the proposed method from the spiked samples were achieved in the range 62.8–108.5%, and RSD ranged from 1.5 to 11.8%.


2009 ◽  
Vol 92 (5) ◽  
pp. 1566-1575 ◽  
Author(s):  
José Fenoll ◽  
Pilar Hellín ◽  
Carmen M Martnez ◽  
Pilar Flores

Abstract An analytical multiresidue method using HPLC/MS/MS with a triple-quadrupole mass spectrometer in the multiple reaction monitoring mode for the simultaneous determination of 54 pesticides in soil has been developed. The procedure involved initial single-phase extraction of soil sample with acetonitrile by sonication, followed by liquidliquid partitioning after addition of NaCl. The average recovery by the HPLC/MS/MS method obtained for these compounds varied from 63.2 to 113.8, with an RSD between 1.9 and 7.1. The method gave good linearity over the assay range of 10500 g/L (except famoxadone, 501000 g/L); the LOD and LOQ for the pesticides varied from 0.02 to 13.2 and from 0.1 to 43.9 g/kg, respectively. The proposed method was used to determine pesticide levels in soil samples from two experimental vineyards and two tomato greenhouses.


2009 ◽  
Vol 92 (3) ◽  
pp. 975-980 ◽  
Author(s):  
Rodrigo Granja ◽  
Alfredo Montes Nio ◽  
Roberto Zucchetti ◽  
Rosario Montes Nio ◽  
Raj Patel ◽  
...  

Abstract Antibiotics are used in apiculture to protect bees against a variety of brood diseases. As a result of the development of resistance to oxytetracycline, erythromycin and tylosin are increasingly used for the prevention and treatment of these diseases. Therefore, Brazilian authorities have added these antibiotics to the National Regulatory Monitoring Program for the control of residues in honey. An analytical method has been developed for the determination of residues of erythromycin and tylosin in honey. The procedure involves solid-phase extraction of diluted honey samples with Bond Elut cartridges, followed by LC/MS with electrospray positive ionization in the multiple reaction monitoring mode. Two characteristic transitions were monitored for both drugs. Average analyte recoveries of erythromycin and tylosin ranged from 99 to 109 from sets of replicate honey samples fortified with drug concentrations of 5, 10, 15, and 20 g/kg. The method decision limits were determined to be 1.27 and 0.59 g/kg for erythromycin and tylosin, respectively. The detection capabilities were 5 and 5.2 g/kg for erythromycin and tylosin, respectively.


2014 ◽  
Vol 68 (11) ◽  
Author(s):  
Wei Liu ◽  
Nan Zhang ◽  
Bing Li ◽  
Sai Fan ◽  
Rong Zhao ◽  
...  

AbstractA simple and fast analytical method for the determination of the main steroidal glycoalkaloids, α-chaconine and α-solanine, in commercial potato crisps, based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged, Safe) extraction and ultra performance liquid chromatography coupled with an electrospray ionization triple-quadrupole tandem mass spectrometer (UPLC-MS/MS) in the multiple reaction monitoring mode was established and validated. The sample preparation procedure involves the extraction of the analytes with acidified acetonitrile and simultaneous liquid-liquid partitioning achieved by an addition of anhydrous magnesium sulfate and sodium acetate without any further clean-up steps. The limits of quantification (LOQs) for α-chaconine and α-solanine were 31 μg kg−1 and 16 μg kg−1 of fresh mass, respectively, at the signal-to-noise ratio (S/Ns) of 10. The method was applied in a survey of the content of α-chaconine and α-solanine in twenty commercial potato crisps from different brands. The results showed that all the products contained α-chaconine and α-solanine in widely varying concentrations. The amount of α-chaconine was higher than that of α-solanine in all samples.


Sign in / Sign up

Export Citation Format

Share Document