柱前手性衍生化-RP-HPLC法拆分D,L-草铵膦  

Chiral Separation of D,L-Glufosinate by RP-HPLC with Chiral Pre-column Derivatization

作　　者：徐建妙[1] 徐永鑫[1] 郑裕国[1] 沈寅初[1] 

机构地区：[1]浙江工业大学生物工程研究所,杭州310014

出　　处：《农药》2013年第3期195-197,201,共4页Agrochemicals

基　　金：浙江省自然科学基金(Y3110391)

摘　　要：[目的]建立柱前手性衍生化-反相高效液相色谱法拆分D,L-草铵膦。[方法]以邻苯二甲醛/N-乙酰基-L-半胱氨酸（OPA/NAC）为手性衍生化试剂,反应生成具有荧光吸收的一对非对映异构体衍生物,采用戴安C18色谱柱,流速1.0 mL/min,50 mmol/L醋酸铵缓冲溶液（pH值5.7）-甲醇（体积比90∶10）流动相,柱温35℃,激发波长350 nm,发射波长450 nm。[结果]L-草铵膦与其光学异构体分离度大于4,最低检测质量浓度为0.1μg/L（S/N≥3）,线性范围为1~100 mg/L（r2为0.9995）,方法重复性好。[结论]采用邻苯二甲醛/N-乙酰基-L-半胱氨酸（OPA/NAC）经柱前手性衍生化-RP-HPLC法可用于L-草铵膦的光学纯度控制。A chiral pre-column derivatization method for optical purity of L-Glufosinate was established.[Methods] Enantiomer was reacted with ortho-phthalaldehyde/N-acety-L-cysteine（OPA/NAC） as chiral derivatization agent to yield a pair of non-chiral derivatives.The chiral separation was carried out on a Dionex C18 column with a mixture of 50 mmol/L ammonium acetate buffer（pH 5.7）-methanol（90∶10,by vol） as mobile phase at a flow rate of 1.0 mL/min.The column temperature was 35 °C with fluorescence detector at Ex 350 nm and Em 450 nm.[Results] The resolution factor was greater than 4 of L-glufosinate and its enantiomer.The limit of detection（LOD） was 0.1 μg/L（S/N≥3）.The linear range of L-glufosinate was 1-100 mg/L with the correlation of 0.999？5.The method had very good repeatability.[Conclusions] The optical purity of L-glufosinate can easily be assessed by RP-HPLC method after being reacted with ortho-phthalaldehyde/N-acety-L-cysteine（OPA/NAC）.

关 键 词：L-草铵膦 手性拆分 柱前衍生化 高效液相色谱法 

分 类 号：TQ450.7[化学工程—农药化工]