鳞翅目昆虫类型Ⅱ性信息素环氧二烯 同分异构体的分离制备
Preparative separation of diene monoepoxides regioisomers mixtures of the Lepidopteran TypeⅡ sex pheromone
罗宗秀 张新忠 崔少伟 李兆群 蔡晓明 边 磊 修春丽 付楠霞 陈宗懋
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DOI:10.7679/j.issn.2095-1353.2022.029
作者单位:中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008;中国农业科学院茶叶研究所,杭州 310008
中文关键词:类型Ⅱ性信息素;环氧二烯同分异构体;分离制备
英文关键词:Type Ⅱ sex pheromone; diene monoepoxides regioisomers; preparative separation
中文摘要:
【目的】 为建立一种适用于鳞翅目昆虫类型Ⅱ性信息素环氧二烯同分异构体的分离制备方法。【方法】 本研究采用半制备高效液相色谱正向系统,结合蒸发光散射检测器和SunFire Silica OBD制备柱,建立了分离制备鳞翅目昆虫类型Ⅱ性信息素方法,制备样品经气相色谱质谱联用仪分析并最终通过田间诱捕试验验证。【结果】 采用0.5%四氢呋喃的正己烷溶液为流动相,流速为7 mL/min,蒸发光散射检测器漂移管温度为40 ℃,在增益设为500的条件下运行,类型Ⅱ性信息素环氧二烯同分异构体的分离效果较好,分离度为2.72-3.10,制备样品单体纯度高,制备样品回收率为80.73%-98.47%;将分离制备的C18环氧二烯同分异构体混合物应用于田间诱捕试验,结果表明本方法制备的顺3,顺9-6,7-环氧十八碳二烯单体结合顺3,顺6,顺9-十八碳三烯可以专一性引诱灰茶尺蠖 Ectropis grisescens,28 d共计诱杀45.33头/诱捕器;制备的顺3,顺6-9,10-环氧十八碳二烯单体结合顺3,顺6,顺9-十八碳三烯可以专一性引诱优美苔蛾Miltochrista striata,28 d共计诱杀44.00头/诱捕器。【结论】 半制备高效液相色谱法是一种简单便利,高效易行的类型Ⅱ性信息素环氧二烯同分异构体的分离制备方法,可满足实验研究与小面积田间应用的需求。
英文摘要:
[Objectives] To establish an effective method for the separation and
preparation of diene monoepoxides
regioisomers mixtures of the Lepidopteran Type Ⅱ sex pheromone. [Methods] The parameters of the method were
established using forward system, semi-preparative, high performance, liquid
chromatography combined with an evaporative light scattering detector and
SunFire Silica OBD preparative column, after which the prepared monomers were
verified by gas chromatography-mass spectrometry and field trapping. [Results] The semi-preparative high performance liquid
chromatography was eluted with 0.5 % tetrahydrofuran in hexane at a flow rate
of 7.0 mL/min with the drift tube temperature of the evaporative light
scattering detector set at 40 ℃ and the gain value set at 500. This
method efficiently separated diene monoepoxides regioisomers mixtures of the Type Ⅱ sex pheromone with a resolution of
2.72-3.10. The purity of the prepared compounds was significant and the recovery rate of prepared samples was
80.73%-98.47%. Field trapping tests confirmed that the prepared Z3, epo6 and
Z9-18:H, in combination with Z3, Z6 and Z9-18:H, specifically attracted Ectropis
grisescens (45.33 moths/trap over 28 d), whereas the prepared Z3, Z6 and
epo9-18:H, in combination with Z3, Z6 and Z9-18:H, specifically
attracted Miltochrista striata (44.00 moths/trap over 28 d). [Conclusion] Semi-preparative
high performance liquid chromatography is a
simple, convenient and efficient method for the separation and preparation of
diene monoepoxides regioisomers mixtures of the Lepidopteran TypeⅡ sex pheromone, and prepared
samples can be used for sex pheromone studies and small-scale field
applications.