印楝素超低容量液剂中印楝素A的HPLC法快速测定
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摘要
建立了高效液相色谱法(HPLC)快速测定印楝素超低容量液剂中有效成分印楝素A的方法.该法采用Agilent C18色谱柱,流动相为乙腈∶5mmol﹒L-1乙酸铵水溶液(40∶60),检测波长218 nm,柱温为35℃.该法的线性范围为10~200μg/m L(R﹥0.998),最低检出限(LOD)为0.5μg/m L,定量限(LOQ)为1.3μg/m L,重复性实验的相对标准偏差(RSD)为3.68%,加标回收率为(102.37±1.78)%.该法适合印楝素超低容量液剂中印楝素A的分析.
The HPLC method was established to quickly determine the azadirachtin A in ultra-low volume. The Agilent C18 column was used with acctonitrile-5 mmol﹒L-1 ammonium acetate(40:60) as mobile phase. The detection wavelength was 218 nm and the column temperature, 35℃. A good linearity was obtained from 10 to 200 μg/m L(R﹥0.998). The limit of detection(LOD) and the limit of quantitation(LOQ) were 0.5 μg/m L and 1.3 μg/m L respectively. The relative standard deviation(RSD) was 3.68% and the recovery rate was 102.37%±SD. The method is suitable for the determination of azadirachtin A.
The HPLC method was established to quickly determine the azadirachtin A in ultra-low volume. The Agilent C18 column was used with acctonitrile-5 mmol﹒L-1 ammonium acetate(40:60) as mobile phase. The detection wavelength was 218 nm and the column temperature, 35℃. A good linearity was obtained from 10 to 200 μg/m L(R﹥0.998). The limit of detection(LOD) and the limit of quantitation(LOQ) were 0.5 μg/m L and 1.3 μg/m L respectively. The relative standard deviation(RSD) was 3.68% and the recovery rate was 102.37%±SD. The method is suitable for the determination of azadirachtin A.
引文
[1]李富根,张宏军,李友顺.植物源农药印楝素的登记与应用[J].农药,2014,53(4):304-306.
[2]徐勇,郭鑫宇,项盛.植物源杀虫剂印楝素研究开发及应用进展[J].现代农药:湖南大学,2014,13(5):31-37.
[3]Heyde J V D,Saxena R C,Schmutterer H.Neem oil and neem extracts as potential insecticides for control of homopterous rice pest[C]//Schmutterer H,Ascher K R S ed.Natural pesticides from the neem tree and other tropical plants,1984:377-390.
[4]Saxena R C,Liquido N J,Justo H D.Neem seed oil,a potential antifeedant for the control of the rice brown planthopper,Nilaparvata lugens[C]//Schmutterer H,Ascher K R S,Rembold H ed.Natural pesticides from the neem tree,1981:171-188.
[5]李永红,张毅,肖卫民,等.比色法测印楝种仁提取物中柠檬苦素类物质的含量[J].西南农业大学学报,2003,25(2):150-156.
[6]武永昆,苏鹏娟,张征,等.印楝素乳油高效液相色谱分析方法研究[J].云南化工,2005,32(6):35-37.
[7]NY/T145-2007中华人民共和国农业行业标准.生物农药中印楝素的测定[S].
[8]叶敏,武永昆,林军,等.悬浮剂中印楝素的高效液相色谱分析方法[J].农药,2006,415(11):760-761.
[9]Paula A M,Brito L F,Caetano K L F N,et al.Ultrasoundassisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A.Juss.(Meliaceae)and its determination by avalidated HPLC-PDA method[J].Talanta,2016,149:77-78.
[10]Forim M R,Cass Q B,Fernandes J B,et al.Simultaneous quantification of azadirachtin and 3-tigloylazadirachtol in Brazilian seeds and oil of Azadirachta indica:application to quality control and marketing[J].Analytical Methods,2010,2(7):860-869.
[11]Tofel K H,Nukenine E N,St?hler M,et al.Degradation of azadirachtin A on treated maize and cowpea and the persistence of Azadirachta indica seed oil on Callosobruchus maculatusand Sitophilus zeamais[J].Journal of Stored Products Research,2016,69:207-212.
[12]郑曦孜.HPLC测定罗氟司特的有关物质[J].光谱实验室,2013,30(6):3122-3126.
[13]高全,姜浩,荀航,等.印楝素类成分对照品的制备与鉴定[J].农药,2015,54(7):490-495.
[2]徐勇,郭鑫宇,项盛.植物源杀虫剂印楝素研究开发及应用进展[J].现代农药:湖南大学,2014,13(5):31-37.
[3]Heyde J V D,Saxena R C,Schmutterer H.Neem oil and neem extracts as potential insecticides for control of homopterous rice pest[C]//Schmutterer H,Ascher K R S ed.Natural pesticides from the neem tree and other tropical plants,1984:377-390.
[4]Saxena R C,Liquido N J,Justo H D.Neem seed oil,a potential antifeedant for the control of the rice brown planthopper,Nilaparvata lugens[C]//Schmutterer H,Ascher K R S,Rembold H ed.Natural pesticides from the neem tree,1981:171-188.
[5]李永红,张毅,肖卫民,等.比色法测印楝种仁提取物中柠檬苦素类物质的含量[J].西南农业大学学报,2003,25(2):150-156.
[6]武永昆,苏鹏娟,张征,等.印楝素乳油高效液相色谱分析方法研究[J].云南化工,2005,32(6):35-37.
[7]NY/T145-2007中华人民共和国农业行业标准.生物农药中印楝素的测定[S].
[8]叶敏,武永昆,林军,等.悬浮剂中印楝素的高效液相色谱分析方法[J].农药,2006,415(11):760-761.
[9]Paula A M,Brito L F,Caetano K L F N,et al.Ultrasoundassisted extraction of azadirachtin from dried entire fruits of Azadirachta indica A.Juss.(Meliaceae)and its determination by avalidated HPLC-PDA method[J].Talanta,2016,149:77-78.
[10]Forim M R,Cass Q B,Fernandes J B,et al.Simultaneous quantification of azadirachtin and 3-tigloylazadirachtol in Brazilian seeds and oil of Azadirachta indica:application to quality control and marketing[J].Analytical Methods,2010,2(7):860-869.
[11]Tofel K H,Nukenine E N,St?hler M,et al.Degradation of azadirachtin A on treated maize and cowpea and the persistence of Azadirachta indica seed oil on Callosobruchus maculatusand Sitophilus zeamais[J].Journal of Stored Products Research,2016,69:207-212.
[12]郑曦孜.HPLC测定罗氟司特的有关物质[J].光谱实验室,2013,30(6):3122-3126.
[13]高全,姜浩,荀航,等.印楝素类成分对照品的制备与鉴定[J].农药,2015,54(7):490-495.