1.Analysis of Oligosaccharide Mapping of Atractylodis Rhizoma from Different Habitats
Likun CHANG ; Wenjin ZHANG ; Ye CAO ; Jian YANG ; Sheng WANG ; Chuanzhi KANG ; Li ZHOU ; Yuefeng WANG ; Chaogeng LYU ; Lanping GUO
Chinese Journal of Experimental Traditional Medical Formulae 2022;28(23):189-196
ObjectiveTo establish a method for the analysis of oligosaccharides in Atractylodes lancea rhizome based on ultra-performance liquid chromatography tandem quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and a method for the quantification of oligosaccharides in A. lancea rhizome based on UPLC-evaporative light scattering detector (ELSD), and to investigate the oligosaccharide characteristics of A. lancea rhizome from different habitats. MethodUPLC-Q-TOF-MS was used to identify the oligosaccharides in A. lancea rhizome with the mobile phase of 0.1% ammonia acetonitrile solution (A)-0.1% ammonia solution (B) for gradient elution (0-0.5 min, 98%A; 0.5-2.0 min, 98%-89%A; 2.0-2.5 min, 89%-86%A; 2.5-5.5 min, 86%-80%A; 5.5-6.5 min, 80%-72%A; 6.5-9.5 min, 72%-63%A; 9.5-14.0 min, 63%-50%A; 14.0-16.0 min, 50%A; 16.0-16.5 min, 50%-98%A; 16.5-20 min, 98%A), the column temperature of 60 ℃ and the flow rate of 0.2 mL·min-1. Electrospray ionization (ESI) was used to collect data in negative ion mode and the detection range was m/z 50-1 500. The qualitative analysis of oligosaccharides was accomplished by retention time, relative molecular weight, primary and secondary MS information of characteristic fragment ions in combination with reference substance information. UPLC-ELSD was employed to determine the contents of nine oligosaccharides in A. lancea rhizome with the mobile phase of 0.1% ammonia acetonitrile solution (A)-0.1% ammonia solution (B) for gradient elution (0-1 min, 98%-75%A; 1-7 min, 75%-70%A; 7-18 min, 70%-55%A; 18-23 min, 55%A; 23-23.5 min, 55%-98%A; 23.5-28 min, 98%A), the drift tube temperature of ELSD was set at 50 ℃. Principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were used to analyze the classification and differential components between A. lancea rhizome from different habitats. ResultA total of 24 oligosaccharides, containing 11 pairs of isomers, were identified from A. lancea rhizome. Among them, compared with samples from Anhui, Chongqing, Nanjing and Shaanxi, the contents of kestose(GF2), 1F-fructofuranosylnystose (GF4), kestohexose (GF5), fructo-oligosaccharide DP10 (GF9) in samples from Maoshan were statistically significant (P<0.05), and the total mass fraction of sucrose (GF1)-GF9 reached 16.47%. The peak area ratio of fructose-fructose oligosaccharide to its isomer sucrose-fructose oligosaccharide was greater than 1 in samples from Maoshan. ConclusionThe types and contents of oligosaccharides in A. lancea rhizome vary greatly among different habitats, and the peak area ratio of fructose-fructose oligosaccharide to sucrose-fructose oligosaccharide >1 may be one of the geoherb characteristics of A. lancea rhizome, which can provide a reference for the development, utilization and quality control of this herb.