ABSTRACT
ObjectiveTo establish the determination for index components in benchmark samples of Erdongtang， and clarify the content and transfer rate rages of index components in 15 batches of benchmark samples， and to explore the quantity transfer of index components of decoction pieces to benchmark samples. MethodFifteen batches of benchmark samples were prepared， the contents of mangiferin， baicalin and glycyrrhizic acid were determined by high performance liquid chromatography （HPLC）-diode array detector （DAD）， the mobile phase was acetonitrile （A）-0.1% formic acid aqueous solution （B） for gradient elution （0-10 min， 10%-17%A； 10-25 min， 17%-19%A； 25-28 min， 19%-25%A； 28-45 min， 25%-33%A； 45-46 min， 33%-45%A； 46-60 min， 45%-55%A）， detection wavelength was set at 254 nm. Contents of timosaponin BⅡ and the sum of protoneodioscin and protodioscin were determined by HPLC-evaporative light scattering detector （ELSD）， the mobile phase was acetonitrile （A）-water （B） for gradient elution （0-20 min， 24%A； 20-25 min， 24%-27%A； 25-33 min， 27%-28%A； 33-36 min， 28%-90%A； 36-41 min， 90%-24%A）. ResultThe methodological verification of the established method was good， which could be used for determination of five index components in benchmark samples. The content ranges of mangiferin， baicalin， glycyrrhizic acid， timosaponin BⅡ， and the sum of protoneodioscin and protodioscin in 15 batches of benchmark samples of Erdongtang were 0.14%-0.23%， 2.40%-3.37%， 0.07%-0.44%， 0.43%-0.95%， and 0.15%-0.47%， the transfer rate ranges of them were 33.90%-52.15%， 84.46%-105.61%， 22.59%-93.86%， 38.07%-61.43%， and 53.28%-96.11%， respectively. ConclusionThe consistencies of transfer rate of mangiferin， baicalin， timosaponin BⅡ and the sum of protoneodioscin and protodioscin （except glycyrrhizic acid） between decoction pieces and benchmark samples of Erdongtang are good， indicates that the transfer rates of 4 index components are stable during the preparation process of benchmark samples， which can provide data support for research and development of the compound preparation of this formula.
ABSTRACT
Objective:There were 92 kinds of compound preparations containing Ophiopogonis Radix in the 2015 edition of Chinese Pharmacopoeia， but there was no effective method to identify these compound preparations. Because Ophiopogonis Radix and Liriopes Radix are similar in appearance， it is easy to be confused in application. The aim of this study was to set up a thin layer chromatography （TLC） to identify compound preparations containing Ophiopogonis Radix and distinguish Ophiopogonis Radix and Liriopes Radix in the forms of decoction pieces and standard decoction. Method:In this study， decoction pieces of Ophiopogonis Radix and Liriopes Radix were collected and separately prepared as standard decoction. TLC was used to qualitatively identify decoction pieces and standard decoction of Ophiopogonis Radix and Liriopes Radix， and compound preparations containing Ophiopogonis Radix. In the TLC， the lower solution of chloroform-methanol-water （65∶35∶10） was selected as the developing agent and 10% sulfuric acid ethanol solution as the chromogenic agent. Result:The resolution of this TLC was good. Decoction pieces， standard decoction and preparations of Ophiopogonis Radix had the same characteristic strips， which were two bright white fluorescent strips under ultraviolet lamp （365 nm）. But these two characteristic strips were not existed in the TLC of decoction pieces and standard decoction of Liriopes Radix. The corresponding components of both of these two strips were identified as mixture containing saponins by LC-MSn， including ophiopogonin Ra， Tb， ophiopogonin D'， borneol glycoside， ophiopogonin C and Liriope muscari baily saponins C. Conclusion:The established TLC method， which has significant advantages such as high specificity and sensitivity， can be applied to the characteristic identification of decoction pieces and standard decoction of Ophiopogonis Radix， the identification of compound preparations containing Ophiopogonis Radix， and the distinction of Ophiopogonis Radix and Liriopes Radix， thus serving as an effective method to qualitatively identify Ophiopogonis Radix and its compound preparations.
ABSTRACT
Objective:To establish the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction. Method:Ten batches of Asparagi Radix standard decoction were prepared. High performance liquid chromatography-evaporative light scattering detection method (HPLC-ELSD) was established for the determination of protodioscin and protoneodioscin in Asparagi Radix decoction pieces and its standard decoction, and the fingerprint detection of Asparagi Radix decoction pieces with acetonitrile-water as mobile phase for gradient elution. UHPLC-LTQ-Orbitrap-MS/MS was used to identify ten main common peaks in the fingerprint with acetonitrile-0.1% formic acid solution as mobile phase for gradient elution, electrospray ionization (ESI) and positive and negative ion mode scanning were employed, the detection range was m/z 100-1 400. Result:The total content of protodioscin and protoneodioscin in Asparagi Radix decoction pieces was 0.41%-0.72%, and their total content in Asparagi Radix standard decoction was 0.33%-0.59%, the transfer rate of these two components was 73.6%-98.3%. The dry extract yield of the standard decoction was 59.0%-73.0%, and its pH was 4.9-5.6. There were 10 common peaks in the fingerprint, and all of them were saponins, including protoneodioscin, protodioscin, aspacochioside A and its isomer, methyl protodioscin, asparagoside F, (25R)-26-O-β-D-glucopyranosyl-furostan-5, 20-diene-3β, 26-diol-3-O-[α-L-rhamnopyranosyl (1→2)]-[β-D-glucopyranosyl (1→4)-α-L-rhamnopyranosyl (1→4)]-β-D-glucopyranoside, 26-O-β-D-glucopyranosyl-furostan-20 (22)-ene-3β, 26-diol-3-O-[α-L-rhamnopyranosyl (1→2)]-[α-L-rhamnopyranosyl (1→4)]-β-D-glucopyranoside, pseudodiosgenin, aspacochioside C. Conclusion:In this paper, the quality evaluation methods of Asparagi Radix decoction pieces and its standard decoction are established, and these methods are stable and feasible, which can provide reference for the quality control of pharmaceutical preparations containing Asparagi Radix.