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目的建立HPLC法测定杀虫丸中木香烃内酯、去氢木香内酯、川楝素和香兰素的含量。方法采用色谱柱:Agilent Epelipse plus C18(250 mm×4.6 mm,5μm),以乙腈-甲醇(1∶2)为流动相A,0.1%醋酸溶液为流动相B进行梯度洗脱;流速为0.9 m L·min~(-1);进样量为20μL;木香烃内酯和去氢木香内酯检测波长为225 nm,川楝素检测波长为215 nm,香兰素检测波长为280 nm。结果木香烃内酯、去氢木香内酯、川楝素和香兰素的线性范围分别为5.87~117.40 mg·L~(-1)(r=0.999 9)、6.71~134.20 mg·L~(-1)(r=0.999 8)、4.87~97.40 mg·L~(-1)(r=0.999 1)和5.15~103.00 mg·L~(-1)(r=0.999 9),线性关系良好;平均加样回收率(n=6)和RSD值分别为98.72%(1.25%)、97.23%(1.41%)、99.50%(1.20%)和97.82%(1.11%)。结论本试验建立的HPLC方法可用于测定杀虫丸中的木香烃内酯、去氢木香内酯、川楝素和香兰素含量,具有一定的准确性、较高的灵敏度和重复性,为评价杀虫丸质量控制提供可靠方法。
OBJECTIVE To establish an HPLC method for the determination of pigeonin, dehydrocostus, toosendanin and vanillin in insecticidal pills. Methods The mobile phase A was eluted with acetonitrile-methanol (1: 2) and the mobile phase consisted of 0.1% acetic acid as mobile phase B on an Agilent Epelipse plus C18 (250 mm × 4.6 mm, 5 μm) L · min ~ (-1). The injection volume was 20μL. The detection wavelength of wood-borneolide and dehydrocostus lactone was 225 nm. The detection wavelength of toosendanin was 215 nm. The detection wavelength of vanillin was 280 nm . Results The linear range of the carnation lactone, dehydrocostus, toosendanin and vanillin were 5.87-117.40 mg · L -1 (r = 0.999 9), 6.71-134.20 mg · L -1 (-1) (r = 0.999 8), 4.87-97.40 mg · L -1 (r = 0.999 1) and 5.15-103.00 mg · L -1 (r = 0.999 9) ; Average recovery (n = 6) and RSD were 98.72% (1.25%), 97.23% (1.41%), 99.50% (1.20%) and 97.82% (1.11%), respectively. Conclusion The HPLC method established in this study can be used to determine the content of woodlocolactone, dehydro-chalcones, toosendanin and vanillin in insecticidal pills with certain accuracy, high sensitivity and repeatability, To evaluate the quality control of insecticidal pills provide a reliable method.