建立了超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定甘草、西洋参、三七、人参、丹参5种中药材中10种三唑类杀菌剂、18种三嗪类除草剂(包括有毒代谢物)残留量的分析方法.采用QuEChERS前处理方法,样品经1％ (v/v)醋酸乙腈提取,乙二胺-N-丙基硅烷(PSA)净化处理,以Shim-pack XR-ODSⅡ(75 mm×2.0 mm)为色谱柱,0.05％ (v/v)甲酸溶液-乙腈为流动相梯度洗脱,在多反应监测(MRM)模式下测定.25种农药及其3种有毒代谢物的定量限(S/N≥10)为0.20～5.52 μg/kg;检出限(S/N≥3)为0.10 ～2.57 μg/kg;在各自的考察浓度范围内线性关系良好(r≥0.999)；在0.20 ～ 55.2 μg/kg添加水平内,平均加标回收率为70.6％ ～ 125.7％,RSD为0.7％ ～14.2％.该方法样品前处理简单、快速、灵敏,可用于中药材中三唑类杀菌剂和三嗪类除草剂农药残留量的快速筛查.
参考文献
| [1] | Wang X C,Jiao X C.Agrochemical(王晓春,焦杏春.农药),2011,50(5):11 |
| [2] | Baranowska I,Barchanska H,Pacak E.Environ Pollut,2006,143:206 |
| [3] | Hernandez F,Sancho J V,Ibanez,et al.Trends Anal Chem,2008,27(10):863 |
| [4] | Lin W X.The Compilation of Residue Limits Standards for Pesticides and Veterinary Drugs in Foodstuffs in the World.Dalian:Dalian Maritime University Press(林维宣.各国食品中农药兽药残留限量规定.大连:大连海事大学出版社),2002 |
| [5] | Zhang X Z,Ma X D,Zhang W G,et al.Chinese Journal of Analytical Chemistry(张新忠,马晓东,张伟国,等.分析化学),2008,36(6):781 |
| [6] | Ren J,Huang C L,Zhao G D,et al.Chinese Journal of Analytical Chemistry(任晋,黄翠玲,赵国栋,等.分析化学),2001,29(8):876 |
| [7] | Li Y Z,Zhang R,Wang H T,et al.Journal of Instrumental Analysis(李育左,张睿,王海涛,等.分析测试学报),2009,28(3):315 |
| [8] | Qi Y,Zhan C R,Zhang X Z,et al.Chinese Journal of Analytical Chemistry(祁彦,占春瑞,张新忠,等.分析化学),2006,34(6):787 |
| [9] | Shen W J,Gui Q W,Yu K Y,et al.Chinese Journal of Chromatography(沈伟健,桂茜雯,余可垚,等.色谱),2009,27(1):91 |
| [10] | Li J G,Wang Y F,Shi J W,et al.Chinese Journal of Chromatography(李继革,王玉飞,施家威,等.色谱),2012,30(3):262 |
| [11] | Wang Y,Jin H Y,Ma S C,et al.J Chromatogr A,2011,1218:334 |
| [12] | Yang X,Zhang H,Liu Y,et al.Food Chem,2011,127:855 |
| [13] | Chen L N,Song F R,Liu Z Q.Journal of Chinese Mass Spectrometry Society(陈丽娜,宋凤瑞,刘志强.质谱学报),2010,31(6):342 |
| [14] | Cao Z Y,Mou R X,Ying X H,et al.Journal of Instrumental Analysis(曹赵云,牟仁祥,应兴华,等.分析测试学报),2010,29(10):1030 |
| [15] | Pihlstr(o)m T,Blomkvist G,Friman P,et al.Anal Bioanal Chem,2007,389:1773 |
| [16] | Yang Y Z,Wu G P,Jiao B N.Modern Agrochemicals(杨玉柱,吴桂苹,焦必宁.现代农药),2007,6(1):34 |
| [17] | AOAC Official Method 2007.01 |
| [18] | EN 15662-2008 |
| [19] | SN/T 0001-1995 |
| [20] | 2002/657/EC |
| [21] | WTO/TBT-SPS Notification and Enquiry of China.Query Database of Japan Positive List(中国技术贸易措施网.日本肯定列表制度查询库).[2012-04-09].http:∥www.tbtsps.com/foodstuff/xlbz/Pages/japan.aspx |
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