文章主要研究了毛发中 9 种毒品的LC-MS/MS定性定量分析方法.毛发样品经过冷冻研磨,甲醇超声,离心取上清液,进样LC-MS/MS分析等实验步骤后,实验数据表明,采用实施例(提取溶剂 17)的方法处理样品,使得 9 种毒品目标物提取效率显著增高,增高率为 18.9％～61.7％.可见,毛发经冷冻研磨,甲醇超声提取 120 min,9 种毒品目标物提取效率有了显著提高,检验结果准确可靠,已应用于实际案例毛发中 9 种毒品的定性定量分析.

Objective: To set up the quantitative method of glycyrrhizic acid in decoctions prepared from various combinations of Baihu Decoction by HPLC and to study the changes of glycyrrhizic acid in eight decoctions.Methods: Different decoctions were prepared and analyzed by L8(27) orthogonal design,the contents of glycyrrhizic acid in each decoction was determined by HPLC.Results: The glycyrrhizic acid content was decreased when Licoroce compatible with other herbs.For Rhizoma Anemarrhenae and Rice,the difference of glycyrrhizic acid was significant(P0.05),for Gypsum,the influence were insignificant,and the interactions between two of three are insignificant too.Conclusion: The content of glycyrrhizic acid in decoction was reduced by Rhizoma Anemarrhenae and Rice.

Objective:To set up the quantitative method of mangiferin in decoctions prepared from various combinations of Baihu decoction by UPLC and to study the changes of mangiferin in eight decoctions.Method:Different decoctions were prepared and analyzed by L8(27) orthogonal design,the content of mangiferin in each decoction was determined by UPLC.Result: The mangiferin content was decreased when Rhizoma Anemarrhenae compatible with other herbs.For rice,the difference of mangiferin was significant(P < 0.05),for Gypsum,Licoroce,the influence was insignificant,and the interactions between two of three were insignificant too.Conclusion: The mangiferin in Baihu decoction could be determinated by UPLC.The methods were simple and rapid,and suitable for the quality control of Baihu decoction.The content of mangiferin in decoction was reduced by rice.

据不完全统计,我国约有80%的中药材来源于人工栽培[1],而中药复方临床疗效的好坏在很大程度上取决于人工栽培的中药材质量的优劣.由于经济效益和社会需求两方面的原因,大多数药农已经把中药材当作普通农作物进行栽培.

Objective:To study the changes of glycyrrhizic acid in eight decoctions.Method:Different decoctions were prepared and analyzed by L8(27) orthogonal design,the content of glycyrrhizic acid in each decoction was determined by UPLC and variance analysis was processed.Result:The glycyrrhizic acid content was decreased when Licorice compatible with other herbs.For Rhizoma Anemarrhenae and Rice,the difference of glycyrrhizic acid was significant(P0.05);for Gypsum,the influence was insignificant,and the interactions between two of three were insignificant too.Conclusion:The content of glycyrrhizic acid in decoction was reduced by Rhizoma Anemarrhenae and Rice.

目的研究冠心苏合丸物质组释放动力学特征。方法以GC-MS法为检测手段,60%乙醇为释放介质,在(37±0.5)℃温度下,采用浆法100 r/min测定同一处方不同厂家生产的和同一厂家生产的不同批号的冠心苏合丸的物质组释放度,以考察不同厂家、不同批号冠心苏合丸物质组释放动力学特征的差异。结果 A厂(批号9012742)、A厂(批号9011245)、A厂(批号8013353)、B厂、C厂和D厂的冠心苏合丸在240 min内物质组的平均累积释放率分别是:104.12%、107.38%、93.79%、69.33%、75.30%和101.36%,释放曲线的Weibull分布参数T50分别为(184.38±19.03)、(186.51±8.65)、(193.38±4.87)、(186.90±10.71)、(246.32±12.90)和(114.23±5.89)min,Td分别为(199.42±22.47)、(202.41±9.16)、(220.64±8.34)、(300.06±34.43)、(374.04±40.57)和(168.07±10.79)min。结论不同厂家的冠心苏合丸物质组释放动力学特征存在显著性差异,同一厂家不同批号间的冠心苏合丸物质组释放动力学特征无显著性差异。

Objective:To study the determination method of catalpol in Radix Rehmanniae by UPLC. Methods:Chromatographic column ACQUITY UPLC BEH RP18 (2.1mm×100 mm,1.7μm),The flow rate is 0.08mL·min-1,The temperature of column is 35℃,The mobile pahase consisted of acetonitrile-water(5:95) and detective wavelength at 210 nm.Results:Catalpol and other pe-aks are separated well and the peak shape was presented well. There is a good linearity within the ran-ge of(3.06 ~18.36)μg with catalpol (Y=4417.4x+860.53,r=0.9997).The average recovery is 100.97%. The RSD is 1.56%(n=6).Conclusion:This method is simple fast accurate and reproducibile. It can be used as the effective detection method of Catalpol in Radix Rehmanniae.

Objective To study the content of calcium ion solubility with different compatibility and to explore the compatible regularity of Baihu Decoction.MethodsThe direct titration was used to study the content of soluble calcium ion of each single herb of Baihu Decoction,their different compatibility,different soaking and boiling time of decoction.ResultsAll of herbs in Baihu Decoction contain calcium.Gypsum had the highest content of calcium,followed by Rhizoma Anemarrhenae and Licoroce,Rice had the lowest.When gypsum compatible with other herbs,the calcium ion content of decoction all descend except gypsum and Licorice compatibility group were slightly increased.The calcium ion solubility of gypsum and Baihu Decoction all increased with extend time of soak.But the solubility of calcium ion decreased with boiling time,especially the group of gypsum declined rapidly.ConclusionExcept the content of calcium ion solubility with gypsum and Licoroce group slightly increase,the other compatibility group content of calcium ion solubility all decreased.The content of calcium ion solubility will enable increased with extending the soaking times,and decreased with extending boiling time.

Objective:To study the soluble calcium ion content of different compatibility of Baihu Decoction and to discuss the compatibility regularity of Baihu Decoction. Method:ICP-AES was used to detect the content of soluble calcium ion of each single and different compatibility herbs in Baihu Decoction. Result:The results showed that all of herbs in Baihu Decoction contained calcium. Gypsum had the highest content of calcium,followed by Rhizoma Anemarrhenae and Licoroce,Rice had the lowest. The calcium ion dissolution content was increased when Gypsum and Licoroce compatibled together; but not influenced by Gypsum and Rice and reduced by Gypsum and Rhizoma Anemarrhenae. Also the calcium ion content was increased when all herbs of Baihu Decoction compatibled together. Conclusion:It reflected the prescription principles of traditional Chinese medicine sufficiently. Gypsum is the monarch drug and Rhizoma Anemarrhenae is the minister drug,both of them have antipyretic effect. Licorice is assistant drug to restrain some Rhizoma Anemarrhenae's negative effects on the calcium ion solubility of gypsum,and increase the antipyretic effect of the monarch drug and minister drug. So the compatibility of traditional Chinese medicine has its own regularity and rationality,it has important guiding significance to the further research on the pharmacological effects of mineral drugs in Chinese herbal compound.