印楝素类成分对照品的制备与鉴定

Preparation and Identification of Chemical Reference Substances of Azadirachtin

[目的]报道一种快速、高效制备印楝素类成分对照品的方法。[方法]采用反相制备高效液相色谱(RP-PHPLC),从印楝粗提物中分离得到10种化合物,并采用NMR和HPLC Q-TOF MS对分离产物进行结构鉴定,通过HPLC检测,外标法或面积归一化法定量。[结果]10种化合物分别是印楝素A(azadirachtin A,AZ-A)、印楝素B(azadirachtin B,AZ-B)、印楝素D(azadirachtin D,AZ-D)、印楝素H(azadirachtin H,AZ-H)、印楝素I(azadirachtin I,AZ-I)以及nimbin、salannin等,10种印楝素类成分对照品的纯度均>98%。[结论]该方法操作简便,可重复进样,适用于制备高纯度印楝素类成分对照品;该对照品可用作印楝素相关产品、制剂质量控制及农产品农药残留检测等实践中的定性、定量依据。

[Aims] A fast and efficient method for preparing chemical reference substances of azadirachtin was studied. [Methods] Ten compounds were isolated from the crude extract of neem seeds by reverse phase preparative high performance liquid chromatography （RP-PHPLC）. The structures of these products were identified by NMR and HPLC Q-TOF MS, and the contents were analysed by HPLC and quantified by external standard method or area normalization method. [Results] The 10 compounds were azadirachtin A （AZ-A）, azadirachtin B （AZ-B）, azadirachtin D （AZ-D）, azadiraehtin H （AZ-H）, azadirachtin I （AZ-I） and nimbin, salannin, etc. The purity of the 10 compounds were all exceed 98%. [Conclusions] The method is simple and repeatable, which is suitable for preparing the high-purity chemical reference substances of azadirachtin. These chemical reference substances can be used as the qualitative and quantitative basis for quality control in the preparation of azadirachtin related products and for pesticide residue detection.