平贝母药材质量控制中适宜测定指标的研究  

Study on index substance for quality control of Bulbus Fritillariae Ussuriensis

作　　者：程显隆[1] 肖新月[1] 夏德豪 张南平[1] 林瑞超[1] 

机构地区：[1]中国药品生物制品检定所,北京100050 [2]湖南省邵阳市药品检验所,长沙422400

出　　处：《药物分析杂志》2008年第1期28-31,共4页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:通过对平贝母中平贝碱甲、贝母素甲、贝母素乙3个单体生物碱成分以及总生物碱测定结果的比较研究,确定可控制平贝母质量的合理测定指标。方法:采用 HPLC—MS 法,色谱柱为 Alltima C_(18)色谱柱(250 mm×4.6 mm,5μm);流动相为乙腈-0.03%二乙胺(30∶70),流速:1 mL·min^(-1);质谱离子源为 ESI;检出模式为正离子检测;电离电压为3.2 kV;电喷雾接口干煤气(N_2)流速为300 L·h^(-1),离子源温度为105℃,锥孔电压为30 V;脱溶剂温度为150℃。选择离子质量数:464.7(平贝碱甲)、432.7(贝母素甲)、430.7(贝母素乙)。测定平贝母中平贝碱甲、贝母素甲、贝母素乙的含量。另以三氯甲烷-甲醇(4∶1)混合溶剂提取总生物碱,以溴麝香草酚蓝比色法在 pH 4.2,紫外吸收波长413 nm 下测定平贝母中总生物碱的含量,结果:LC—MS 法测定平贝母中平贝碱甲、贝母素甲、贝母素乙的含量分别为5～19,1～3,2～3μg·g^(-1);溴麝香草酚蓝比色法测定总生物碱含量以贝母素乙计为600～1000 μg·g^(-1)。结论:平贝母中单-生物碱成分含量太低,不宜作为平贝母药材的质量控制指标,以溴麝香草酚蓝比色法测定总生物碱含量可更客观反映平贝母药用物质情况,更适用于平贝母药材的质量控制。Objective： To observe the comparative result between the content of pingpeimine A, peimine, peiminine and the content of total alkaloids in Bulbus Fritillariaee Ussuriensis. and to select the reasonable index substance for quality control of Bulbus Ffitillariae Ussuriensis. Method： The liquid chromatography - mass spectrometry method was developed to determine the content of pingpeimine A, peimine, peiminine in Bulbus Fritillariae Ussuriensis. The HPLC separation was performed on an Alltima Cls （250 mm× 4.6 mm,5 μm ） column, using acetonitrile -water （ diethylamine 0.03% ） （30： 70） as mobile phase, with a flow rate of 1 mL · min ^-1, and ESI ^＋ was employed, the sample was analyzed in the positive- ion mode. Capillary voltage was 3.20 kV, desolvation gas flow was 300 L ·h^-1,the cone voltage was 30 V, desolvation temperature was 150 ℃, source temperature was 105 ℃, selective ion： 464.7 （ pingpeimine A） ,432.7 （peimine） ,430.7 （peiminine）. And bromothymol blue colorimetric method was developed to determine the content of total alkaloids in pH 4.2 and UV 413 nm. Results： The contents of pingpeimine A, peimine, and peiminine were 5 - 19,1 - 3, and 2 - 3 μg · g ^- 1 respectively by LC - MS ; The content of total alkaloids was 600 - 1000 μg · g^-1 in Bulbus Ffitillariae Ussuriensis by bromothymol blue colorimetric method. Conclusions ： The single alkaloid is not suitable for the index substance of quality control of Bulbus Fritillariae Ussuriensis. The determination of total alkaloids by bromothymol blue colorimetric method can be used for quality control of Bulbus Fritillariae Ussuriensis.

关 键 词：平贝母 高效液相色谱-质谱法 溴麝香草酚蓝比色法 总生物碱 

分 类 号：R917[医药卫生—药物分析学]