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采用超临界流体色谱,以超临界二氧化碳(CO2)作为流动相,研究了6种手性三唑类杀菌剂(苄氯三唑醇、联苯三唑醇、叶菌唑、乙环唑、糠菌唑和醚唑)在Chiralcel OD-H手性色谱柱上的对映体分离。考察了不同改性剂种类(甲醇、乙醇、异丙醇)、体积分数(0~15%)以及系统背压(13~17 MPa)对分离效果的影响,并与其在Sino-Chiral OJ和Chiralpak IB手性色谱柱上的分离效果进行了比较。结果表明:单独以超临界CO2为流动相时,6种三唑类杀菌剂的保留时间均大于60 min,而添加了醇类改性剂后其在40 min内均得到了洗脱。苄氯三唑醇、联苯三唑醇、叶菌唑和糠菌唑在柱温为34℃、系统背压为15 MPa、流动相流速为2 m L/min时,在20 min内均实现了基线分离(Rs≥1.5);优化改性剂(体积分数)分别为3%乙醇、13%乙醇、6%甲醇和7%乙醇。Chiralcel OD-H柱对6种供试杀菌剂的手性识别效果优于Sino-Chiral OJ和Chiralpak IB柱,但对映体分离时间要长10~20 min。
Using supercritical fluid chromatography and supercritical carbon dioxide (CO2) as the mobile phase, the effects of six chiral triazole fungicides (benazlazol, tribenzotriazole, metconazole, Enzazole and fenfluconazole) on Chiralcel OD-H chiral column. The effect of different modifier species (methanol, ethanol, isopropanol), volume fraction (0-15%) and system backpressure (13-17 MPa) on the separation efficiency was investigated and compared with that of Sino-Chiral OJ and Chiralpak IB chiral column on the separation of the results were compared. The results showed that when the supercritical CO2 was used as the mobile phase alone, the retention times of all the six triazole fungicides were all greater than 60 min. After the addition of the alcohol modifier, they all eluted within 40 min. Tribenzotriazole, tribenzotriazole, metconazole and shikisoprazole were all achieved within 20 min at a column temperature of 34 ° C, a system back pressure of 15 MPa and a mobile phase flow rate of 2 mL / min Baseline separation (Rs≥1.5); optimized modifiers (volume fraction) were 3% ethanol, 13% ethanol, 6% methanol and 7% ethanol, respectively. Chiralcel OD-H column was superior to Sino-Chiral OJ and Chiralpak IB for chiral recognition of the six tested fungicides, but the enantiomeric separation time was 10 ~ 20 min.