气相色谱-四极杆-飞行时间质谱法快速筛查黄芪药材中27种除草剂残留
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摘要
目的建立了气相色谱-四极杆-飞行时间质谱(GC-Q-TOF/MS)对黄芪中27种除草剂农药残留量的分析方法。方法样品以含1%乙酸的乙腈提取、Qu ECh ERS技术净化,采用气相色谱-四极杆-飞行时间质谱对27种除草剂进行测定。通过保留时间、一级质谱全扫描离子定性、并结合MS/MS模式对阳性样品进行二次确证,特征离子外标法定量。结果 27种除草剂在20~1000μg/L线性范围内均呈良好线性关系,相关系数大于0. 99,检出限为2. 2~23. 9μg/kg。在20,100,200μg/kg三个添加水平下的平均回收率为71. 7%~109. 4%,相对标准偏差(RSD)为2. 1%~13. 6%。结论该方法简便、快速、灵敏、准确,为黄芪药材中27种除草剂残留量的测定提供可靠依据。
Objective A method has been developed for the rapid screening of 27 herbicides in Astragalus mongholicus. Methods Samples were extracted with acetonitrile( containing 1% acetic acid),then cleaned up with Qu ECh ERS,and finally analyzed by gas chromatography coupled with quadrupole-time of flight mass spectrometry. Qualitation by retention time,first mass scan,and quantitation was performed with the external standard method. Results The method showed good linearity over the range of 20 ~1000 μg/L with correlation coefficients of all above 0. 99. The limits of detection was 2. 2 ~ 23. 9 μg/kg. The average recovery range of three fortified levels( 20,100,200 μg/kg) is 71. 7% ~ 109. 4%,with RSDs of 2. 1%-13. 6%. Conclusion The proposed method is simple,rapid and sensitive,suitable for the rapid screening of 27 herbicides in Astragalus mongholicus.
Objective A method has been developed for the rapid screening of 27 herbicides in Astragalus mongholicus. Methods Samples were extracted with acetonitrile( containing 1% acetic acid),then cleaned up with Qu ECh ERS,and finally analyzed by gas chromatography coupled with quadrupole-time of flight mass spectrometry. Qualitation by retention time,first mass scan,and quantitation was performed with the external standard method. Results The method showed good linearity over the range of 20 ~1000 μg/L with correlation coefficients of all above 0. 99. The limits of detection was 2. 2 ~ 23. 9 μg/kg. The average recovery range of three fortified levels( 20,100,200 μg/kg) is 71. 7% ~ 109. 4%,with RSDs of 2. 1%-13. 6%. Conclusion The proposed method is simple,rapid and sensitive,suitable for the rapid screening of 27 herbicides in Astragalus mongholicus.
引文
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[14]李继革,施家威,王玉飞.固相萃取-气相色谱-串联质谱法测定大米中10种除草剂[J].中国卫生检验杂志,2016,26(10):1388.
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[17]祁晓霞,董宇,单晨啸,等.基于UFLC-Q-TOF/MS分析黄芪-丹参药对化学成分研究[J].南京中医药大学学报,2017,33(1):93.
[18]李春苗,胡雪艳,范春林,等.GC-Q-TOF/MS快速筛查测定半夏中322种农药及化学污染物残留[J].分析测试学报,2017,36(4):431.
[19]李晓颍,张红医,常巧英,等.气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留[J].色谱,2014,32(3):268.
[20]Lozowicka B,Rutkowska E,Jankowska M.Influence of QuEChERSmodifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD[J].Environ Sci Pollut Res,2017,24(8):7124.
[21]陈晓水,边照阳,唐纲岭,等.气相色谱-串联质谱技术分析烟草中的132种农药残留[J].色谱,2012,30(10):1043.
[22]刘胜男,卫星,巩卫东.Qu EChERS方法在检测分析中的应用研究进展[J].食品研究与开发,2013,34(10):133.
[23]周蓉,曹赵云,赵肖华,等.分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留[J].分析测试学报,2017,36(1):67.
[2]汪雪飞,夏润玺,王雅婷,等.几种常用除草剂对家蚕生长发育的影响[J].安徽农业科学,2017,45(2):174.
[3]傅建炜,史梦竹,李建宇,等.草甘膦对草鱼、鲢鱼和鲫鱼的毒性[J].生物安全学报,2013,22(2):119.
[4]Astiz M,de Alaniz MJ,Marra CA.Antioxidant defense system in rats simultaneously intoxicated with a agrochemicals[J].Environ Toxicol Pharmacol,2009,28(3):465.
[5]范甜甜,杨治峰,张振玲.除草剂草甘膦毒作用的研究进展[J].环境与健康杂志,2017,34(1):91.
[6]张越,全焕荣,段志文,等.阿特拉津对小鼠微核及精子畸形率的影响[J].沈阳医学院学报,2000,3(2):72.
[7]滕国琴,戴璇颖,徐世清.阿特拉津对家蚕生殖发育的影响[J].生态毒理学报,2007,3(2):315.
[8]杨婉珍,康传志,纪瑞锋,等.中药材残留农药情况分析及其标准研制的思考[J].中国中药杂志,2017,42(12):2284.
[9]中华人民共和国药典委员会.中华人民共和国药典,四部[S].北京:中国医药科技出版社,2015:209.
[10]European Directorate for Quality Medicines.Europe pharmacopoeia[S].8th edition.2013
[11]The United States Pharmacopeial Convention.The united statespharmacopoeia[S].36th Edition.2013
[12]田宏哲,白雪松,苑馨方,等.气相色谱-电子捕获检测器同时测定瓜果类蔬菜中15种除草剂残留[J].农药学学报,2016,18(5):625.
[13]乔丹,刘小静,韩典峰,等.气相色谱-质谱法测定动物源性水产品中16种除草剂[J].渔业科学进展,2017,38(4):172.
[14]李继革,施家威,王玉飞.固相萃取-气相色谱-串联质谱法测定大米中10种除草剂[J].中国卫生检验杂志,2016,26(10):1388.
[15]杨益林,潘艳坤,周玉薇,等.液相色谱-串联质谱法测定甘蔗中10种除草剂的残留量[J].理化检验-化学分册,2017,53(5):507.
[16]Kaczyński P.Large-scale multi-class herbicides analysis in oilseeds by rapid one-step Qu EChERS-based extraction and cleanup method using liquid chromatography-tandem mass spectrometry[J].Food Chem,2017,230:411.
[17]祁晓霞,董宇,单晨啸,等.基于UFLC-Q-TOF/MS分析黄芪-丹参药对化学成分研究[J].南京中医药大学学报,2017,33(1):93.
[18]李春苗,胡雪艳,范春林,等.GC-Q-TOF/MS快速筛查测定半夏中322种农药及化学污染物残留[J].分析测试学报,2017,36(4):431.
[19]李晓颍,张红医,常巧英,等.气相色谱-四极杆飞行时间质谱准确鉴定常见水果蔬菜中的农药残留[J].色谱,2014,32(3):268.
[20]Lozowicka B,Rutkowska E,Jankowska M.Influence of QuEChERSmodifications on recovery and matrix effect during the multi-residue pesticide analysis in soil by GC/MS/MS and GC/ECD/NPD[J].Environ Sci Pollut Res,2017,24(8):7124.
[21]陈晓水,边照阳,唐纲岭,等.气相色谱-串联质谱技术分析烟草中的132种农药残留[J].色谱,2012,30(10):1043.
[22]刘胜男,卫星,巩卫东.Qu EChERS方法在检测分析中的应用研究进展[J].食品研究与开发,2013,34(10):133.
[23]周蓉,曹赵云,赵肖华,等.分散固相萃取-分散液液微萃取/气相色谱-串联质谱法测定蔬菜中19种有机磷农药残留[J].分析测试学报,2017,36(1):67.