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2 Acta Chromatographica

2 2024

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Ultra-rapid determination of andrographolide and dehydroandrographolide in Andrographis Herba by solid phase extraction and liquid chromatography with mass spektrometry

100%

Qian Z. , Chen J. , Lei Q. , Li D. , Tan G. , Xie J. , Li W.

Acta Chromatographica

2024

tom Vol. 36, no. 3

279-–285

An ultra-rapid analytical method for determination of andrographolide and dehydroandrographolide in Andrographis Herba (AH) was developed by liquid chromatography with mass spectrometry (LC-MS). The sample was ultrasonically extracted with 10 mL 40% (v/v) methanol, and then purified with a C18 solid phase extraction column. The LC separation was performed on a Poroshell 120 EC-C18 column (3032.1 mm, 2.7 μm) and eluted with 0.5 mmol L1 ammonium acetate aqueous solution and acetonitrile (65:35) at a flow rate of 0.7 mL min1, and detected by mass spectrometry (MS). The LC-MS analytical time was less than 1 min. The new developed method presented a good linearity (r > 0.9900), precision and repeatability (RSD < 2.0%). The recoveries for andrographolide and dehydroandrographolide were 93.5% (RSD 5 2.2%) and 97.7% (RSD 5 2.4%), respectively. The developed method was successfully applied in determination of andrographolide and dehydroandrographolide in seven batches of AH samples, and the contents of analytes in all samples were complied with the relative acceptance criteria in Chinese Pharmacopeia (>0.8%). This new developed LC-MS method is an ultrarapid assay method for AH, which will help to improve the efficiency and reduce the cost of AH sample test.

A simple, rapid, sensitive and eco-friendly LC-MS/MS method for simultaneous determination of free cordycepin and isocordycepin in 10 different kinds of Cordyceps

84%

Li W. , Qian Z. , Zou Y. , Tan G. , Li W. , Lei Q. , Li R. , Lan D.

Acta Chromatographica

2024

tom Vol. 36, no. 1

59--66

A simple, rapid, sensitive and eco-friendly liquid chromatography tandem mass spectrometry (LC-MS/MS) method was developed for simultaneous determination of free cordycepin (3′-deoxyadenosine) and isocordycepin (2′-deoxyadenosine) in 10 kinds of Cordyceps samples. The samples were prepared by ultrasonic extraction at 75 °C for 30 min with boiling water as the extraction solvent. The LC separation was performed on an Agilent poroshell 120 SB-Aq C18 column (3.0 × 50 mm, 2.7 μm) in isocratic mode with an eco-friendly mobile phase (2% ethanol containing 0.2% acetic acid) at a flow rate of 0.6 mL min⁻¹, and detected by MS/MS in positive mode with multiple reaction monitoring (MRM). The developed method showed good linearity (r > 0.9990), sensitivity (LODs = 0.04 pg, LOQ = 0.1 pg), precision (RSD ≤ 3.8%) and stability (RSD ≤ 3.6%). The recoveries of developed method were 94.4–109.5% (RSD ≤ 5.5%). Compared with reported methods, the current method was rapid (less than 35% analytical time), sensitive (more than 5 folds), and eco-friendly (less than 10 μL harmful organic solvent). 10 different kinds of Cordyceps samples (40 batches) were tested by the developed method. Codycepin was only found in Cordyceps millitaris and C. millitaris fruiting body, and isocordycepin was detected in Cordyceps sinensis and other 6 Cordyceps samples. The developed method would be an improved method for the quality evaluation of Cordyceps samples.