UPLC-MS/MS法同时测定裸花紫珠药材中9种农药残留
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摘要
目的采用固相萃取(SPE)前处理技术净化样品,建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定裸花紫珠药材中9种农药残留的方法。方法裸花紫珠样品用乙腈提取,通过Cleanet-TPH固相萃取柱净化,采用安捷伦1290~6460超高效液相色谱质谱联用仪测定,流动相为乙腈-水(含0.1%甲酸),扫描方式为多反应离子监测(MRM)模式。结果多菌灵、敌百虫、敌敌畏、灭线磷、倍硫磷、甲拌磷、丙溴磷、辛硫磷、丁硫克百威等9种被测物质的线性关系良好,相关系数为0.997 8~0.999 7,各农药的定量限为0.003~3.1μg/kg,测试精密度和重复性良好,RSD值均<3.0%;高、中、低3个浓度的样品加标回收率范围为92.7%~103.9%。3批裸花紫珠样品检出了多菌灵、敌百虫、辛硫磷等3种农药残留。结论所建立的方法简便、准确度及灵敏度高、分析速度快、专属性好,可用于裸花紫珠药材中9种农药残留的测定。
Objective To develop a method for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) after purification of samples by solid phase extraction(SPE) pretreatment. Methods The samples of Callicarpa nudiflora were extracted with acetonitrile, purified by Cleanet-TPH solid phase extraction column, and analyzed by UPLC-MS/MS(Agilent1290-6460); the mobile phase was acetonitrile-water(containing 0.1% formic acid) and the scanning mode was multiple reaction monitoring(MRM). Results The linear relationships of 9 kinds of tested substances was good, including carbendazim, dipterex, dichlorvos, chlorpyrifos, fenthion, phorate, profenofos, phoxim and carbosulfan; the correlation coefficient(r) was between 0.997 8 and 0.999 7; the limit of quantification(LOQ) of each pesticide was in the range of0.003~3.1 μ g/kg, the test precision and repeatability were good, and the RSD values were all<3.0%. The recovery of high, medium and low concentrations of the samples ranged from 92.7% to 103.9%. Three kinds of pesticide residues such as carbendazim, dipterex and phoxim were detected in 3 batches of Callicarpa nudiflora sample. Conclusion The method established in this study is simple, accurate and sensitive, fast in analysis and good in specificity. It can be used for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora.
Objective To develop a method for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora by ultra-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS) after purification of samples by solid phase extraction(SPE) pretreatment. Methods The samples of Callicarpa nudiflora were extracted with acetonitrile, purified by Cleanet-TPH solid phase extraction column, and analyzed by UPLC-MS/MS(Agilent1290-6460); the mobile phase was acetonitrile-water(containing 0.1% formic acid) and the scanning mode was multiple reaction monitoring(MRM). Results The linear relationships of 9 kinds of tested substances was good, including carbendazim, dipterex, dichlorvos, chlorpyrifos, fenthion, phorate, profenofos, phoxim and carbosulfan; the correlation coefficient(r) was between 0.997 8 and 0.999 7; the limit of quantification(LOQ) of each pesticide was in the range of0.003~3.1 μ g/kg, the test precision and repeatability were good, and the RSD values were all<3.0%. The recovery of high, medium and low concentrations of the samples ranged from 92.7% to 103.9%. Three kinds of pesticide residues such as carbendazim, dipterex and phoxim were detected in 3 batches of Callicarpa nudiflora sample. Conclusion The method established in this study is simple, accurate and sensitive, fast in analysis and good in specificity. It can be used for the determination of 9 pesticide residues in medicinal Callicarpa nudiflora.
引文
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[12]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 23200.11-2016桑枝、金银花、枸杞子和荷叶中413种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.
[13]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 23200.13-2016茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.
[2]董琳,张小菁,刘明生.裸花紫珠5-羟基-3,7,3',4'-四甲氧基黄酮抗炎作用研究[J].海南医学院学报,2014,20(11):1460.
[3]刘小芬,李顺祥.裸花紫珠研究进展[J].中南药学,2015,13(4):396-402.
[4]马燕春,张旻,徐文彤,等.裸花紫珠化学成分及细胞毒活性研究[J].中国中药杂志,2014,39(16):3094.
[5]海南省质量技术监督局.DB46/T 354-2016裸花紫珠采种及育苗技术规程[S].海口,2016.
[6]国家对外贸易经济合作部.药用植物及制剂进出口绿色行业标准[S].北京:中国标准出版社,2001.
[7]康传志,郭兰萍,周涛,等.中药材农残研究现状的探讨[J].中国中药杂志,2016,41(2):155-159.
[8]钱韵旭.国外新农残标准对中药出口的影响及对策研究[D].沈阳:沈阳药科大学,2014.
[9]楼步青,徐鸿华.南药规范化种植调研及发展策略[J].时珍国医国药,2011,22(8):1999-2000
[10]苏靖,戴荣继.液质联用技术在中药研究中的应用[J].生命科学仪器,2014,12(2):40.
[11]罗芬.液-质联用技术在中药分析中的应用[J].亚太传统医药,2014,10(11):52.
[12]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 23200.11-2016桑枝、金银花、枸杞子和荷叶中413种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.
[13]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB 23200.13-2016茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法[S].北京:中国标准出版社,2016.