Hoke S H, Cooks R G, Chang C J, Kelly R C, Qualls S J, Alvarado B, McGuire M T, Snader K M
Department of Chemistry, Purdue University, West Lafayette, IN 47907.
J Nat Prod. 1994 Feb;57(2):277-86. doi: 10.1021/np50104a013.
A tandem mass spectrometric (ms/ms) method using desorption chemical ionization is described for the quantitation of taxol [1], cephalomannine [2], and baccatin III [3] found in Taxus brevifolia bark and needle extracts. A parent ion scan was used to simultaneously determine the weight percentages of 1-3 in bark and needle samples by the method of standard addition. In an alternative experiment, the concentration of 1 in the same samples was determined by ms/ms using trideuterated 10-acetyltaxol [7a] as an internal standard. High-performance liquid chromatography (hplc) was also used to determine the weight percentages of 1-3 in the same T. brevifolia bark and needle extracts with an external standard. The ms/ms method of quantitation by internal standard is the best overall method of analysis examined. With this method, 1 was quantitated in the T. brevifolia extracts at the low picomole level with a relative standard deviation of 17% or better for all samples analyzed with an analysis time of less than five min per sample. The precision, level of quantitation, and speed of analysis of the three methods of taxane quantitation are compared.
本文描述了一种使用解吸化学电离的串联质谱(MS/MS)方法,用于定量测定短叶红豆杉树皮和针叶提取物中的紫杉醇[1]、三尖杉宁碱[2]和巴卡亭III[3]。采用母离子扫描,通过标准加入法同时测定树皮和针叶样品中1-3的重量百分比。在另一个实验中,使用氘代10-乙酰紫杉醇[7a]作为内标,通过MS/MS测定相同样品中1的浓度。还使用高效液相色谱(HPLC)以外标法测定相同短叶红豆杉树皮和针叶提取物中1-3的重量百分比。内标法定量的MS/MS方法是所研究的最佳总体分析方法。使用该方法,在短叶红豆杉提取物中,1在低皮摩尔水平下进行定量,对于所有分析的样品,相对标准偏差为17%或更低,每个样品的分析时间少于5分钟。比较了三种紫杉烷定量方法的精密度、定量水平和分析速度。