Determination of taxanes in Taxus brevifolia extracts by tandem mass spectrometry and high-performance liquid chromatography.
Determination of taxanes in Taxus brevifolia extracts by tandem mass spectrometry and high-performance liquid chromatography.
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采用串联质谱和高效液相色谱法测定短叶红豆杉提取物中的紫杉烷类化合物。
DOI：
10.1021/np50104a013
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发表时间：
1994
影响因子：
5.1
通讯作者：
Snader,KM
中科院分区：
文献类型：
--
作者：
Hoke2nd,SH;Cooks,RG;Chang,CJ;Kelly,RC;Qualls,SJ;Alvarado,B;McGuire,MT;Snader,KM
建立了一种解吸化学电离串联质谱仪(MS/MS)测定短叶红豆杉树皮和针叶提取物中紫杉醇[1]、头孢甘露[2]和巴卡菌素III[3]的方法。用标准加入法同时测定了树皮和针叶样品中1-3的重量百分比。在另一种实验中，用三氢代10-乙酰紫杉醇[7a]作为内标，用MS/MS法测定相同样品中1的浓度。采用高效液相色谱(HPLC法)测定了同一药材、短叶树皮提取物和针叶提取物中1-3的重量百分比，并与外标进行了比较。内标MS/MS法定量是所考察的最佳综合分析方法。用该方法对所有样品在每个样品分析时间小于5min的情况下，以较低的皮摩尔水平定量1，其相对标准偏差为17%或更好。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。
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 internalstandard 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.