UHPLC-MS/MS Determination of 4 Pheulurea Herbicides in Water
摘 要
取水样50.0 mL,加盐酸调节pH至3.0,用吡咯烷酮基和二乙烯基苯修饰的磁性纳米材料50.0 mg振荡吸附20 min。乙腈3.0 mL洗脱后,将洗脱液离心5 min,过0.22 μm有机滤膜,氮吹至近干,用甲醇-0.1%(体积分数)甲酸(60+40)混合液定容至1 mL。所得溶液进行超高效液相色谱分离,以XDB-C18反相色谱柱为固定相,以不同体积比的甲醇和0.1%(体积分数)甲酸溶液的混合液为流动相梯度洗脱。质谱分析采用多反应监测模式。4种苯脲类除草剂的质量浓度在0.05~5.0 μg·L-1内与其峰面积呈线性关系,检出限(3.143s)为12.5~16.4 ng·L-1。按标准加入法进行回收试验,回收率为83.7%~107%,测定值的相对标准偏差(n=6)均小于8.5%。
Abstract
The sample (50.0 mL) was adjusted pH to 3.0 with HCl solution, and adsorbed by swirling for 20 min with 50.0 mg of magnetic nanomaterials modified with ketopyrrolidine and divinylbenzene. After elution with 3.0 mL of acetonitrile, the eluent was centrifuged for 5 min, and filtered through 0.22 μm organic filter membrane. The filtrate was dried by N2-blowing, and made up its volume to 1 mL, with a mixture of methanol-0.1% (φ) formic acid (60+40). The sample solution was separated by UHPLC using XDB-C18 reversed-phase chromatographic column as stationary phase, and mixtures of methanol and 0.1% (φ) formic acid solution in various volumic ratios as mobile phase in gradient elution. MRM was adopted in MS. Linear relationships between values of peak area and mass concentration of 4 pheulurea herbicides were found in the range of 0.05-5.0 μg·L-1, with detection limits (3.143s) in the range of 12.5-16.4 ng·L-1. Test for recovery was made by standard addition method, giving results in the range of 83.7%-107%, with RSDs (n=6) all less than 8.5%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201801016
所属栏目 工作简报
基金项目 江苏省高校自然科学研究重大项目(15KJA610003);苏州科技大学校青年基金(341511201)
收稿日期 2016/12/29
修改稿日期
网络出版日期
作者单位点击查看
备注金主晶(1991-),女,江苏南通人,硕士研究生,研究主方向为环境污染物分析检测
引用该论文: JIN Jing,GU Haidong,GAO Shiqian,WANG Junxia,ZHANG Zhanen. UHPLC-MS/MS Determination of 4 Pheulurea Herbicides in Water[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(1): 77~81
金晶,顾海东,高仕谦,王俊霞,张占恩. 超高效液相色谱-串联质谱法测定水中4种苯脲类除草剂的含量[J]. 理化检验-化学分册, 2018, 54(1): 77~81
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】刘恩梅,生威,韩静,等.苯脲类除草剂残留检测方法研究进展[J].食品与机械, 2011,27(3):160-164.
【2】支建梁,牟仁祥,陈铭学,等.柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂[J].色谱, 2008,26(1):93-97.
【3】GONCALVESA C, ALPENDURADA M F. Solid-phase micro-extraction-gas chromatography-(tandem) mass spectrometry as a tool for pesticide residue analysis in water samples at high sensitivity and selectivity with confirmation capabilities[J]. Journal of Chromatography A, 2004,1026(1/2):239-250.
【4】李向梅,周建科,付艳芳.低温冷冻萃取-色谱法测定芝麻糊中苯脲除草剂[J].化学研究与应用, 2014,26(1):145-148.
【5】赵进英,辛暨华,郭英娜,等.固相富集萃取-高效液相色谱法分离检测水中3种苯脲除草剂[J].分析化学, 2004,32(7):939-942.
【6】LI F S, MARTENS D, KETTRUP A. Simultaneous determination of sixteen phenylurea herbicides in water by high performance liquid chromatography and solid phase extraction[J]. Chinese Journal of Chromatography, 2001,19(6):534-537.
【7】QUIRINO J P, INOUE N, TERABE S. Reversed migration micellar electrokinetic chromatography with off-line and on-line concentration analysis of phenylurea herbicides[J]. Journal of Chromatography A, 2000,892(1/2):187-194.
【8】张娟.环境中苯脲类除草剂的分析和处理[D].南京:南京工业大学, 2005.
【9】LI Y T, GEORGE J E, CHRISTINA L M, et al. Complicance analysis of phenylurea and related compounds in drinking water by liquid chromatography/electrospray ionization/mass spectrometry coupled with solid-phase extraction[J]. Journal of Chromatography A, 2006,1134(1/2):170-176.
【10】SAGRATINI G, MAÑES J, GIARDINÁ D, et al. Analysis of carbamate and phenylurea pesticide residues in fruit juices by solid-phase microextraction and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2007,1147(2):135-143.
【11】CHOU T Y, LIN S L, FUH M R. Determination of phenylurea herbicides in aqueous samples using partitioned dispersive liquid-liquid microextration[J]. Talanta, 2009,80(2):493-498.
【12】陈园,张丽君,顾海东,等.分散固相萃取-UHPLC-MS/MS法测定水中5种苯脲类除草剂[J].化学试剂, 2016,38(3):245-248.
【13】HE Z Y, LIU D H, LI R H, et al. Magnetic solid-phase extration of sulfonylurea herbicides in environmental water samples by Fe3O4@dictadecyl dimethyl ammonium chloride@silica magnteic particles[J]. Analytica Chimica Acta, 2012,747:29-35.
【14】连丽丽,郭亭秀,吴玉清,等.磁性固相萃取-液相色谱法测定环境水样中痕量的微囊藻毒素[J].分析化学, 2015,43(12):1876-1881.
【15】白沙沙,李芝,臧晓欢,等.磁性石墨烯固相萃取-分散液液微萃取-气相色谱法测定水和绿茶中酰胺类除草剂残留[J].分析化学, 2013,41(8):1177-1182.
【16】张贵江,臧晓欢,周欣,等.磁性石墨烯纳米粒子固相萃取与气相色谱-质谱相结合测定环境水样中的三嗪类除草剂[J].色谱, 2013,31(11):1071-1075.
【2】支建梁,牟仁祥,陈铭学,等.柱后紫外光解荧光衍生液相色谱法测定蔬菜中残留的15种苯脲除草剂[J].色谱, 2008,26(1):93-97.
【3】GONCALVESA C, ALPENDURADA M F. Solid-phase micro-extraction-gas chromatography-(tandem) mass spectrometry as a tool for pesticide residue analysis in water samples at high sensitivity and selectivity with confirmation capabilities[J]. Journal of Chromatography A, 2004,1026(1/2):239-250.
【4】李向梅,周建科,付艳芳.低温冷冻萃取-色谱法测定芝麻糊中苯脲除草剂[J].化学研究与应用, 2014,26(1):145-148.
【5】赵进英,辛暨华,郭英娜,等.固相富集萃取-高效液相色谱法分离检测水中3种苯脲除草剂[J].分析化学, 2004,32(7):939-942.
【6】LI F S, MARTENS D, KETTRUP A. Simultaneous determination of sixteen phenylurea herbicides in water by high performance liquid chromatography and solid phase extraction[J]. Chinese Journal of Chromatography, 2001,19(6):534-537.
【7】QUIRINO J P, INOUE N, TERABE S. Reversed migration micellar electrokinetic chromatography with off-line and on-line concentration analysis of phenylurea herbicides[J]. Journal of Chromatography A, 2000,892(1/2):187-194.
【8】张娟.环境中苯脲类除草剂的分析和处理[D].南京:南京工业大学, 2005.
【9】LI Y T, GEORGE J E, CHRISTINA L M, et al. Complicance analysis of phenylurea and related compounds in drinking water by liquid chromatography/electrospray ionization/mass spectrometry coupled with solid-phase extraction[J]. Journal of Chromatography A, 2006,1134(1/2):170-176.
【10】SAGRATINI G, MAÑES J, GIARDINÁ D, et al. Analysis of carbamate and phenylurea pesticide residues in fruit juices by solid-phase microextraction and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2007,1147(2):135-143.
【11】CHOU T Y, LIN S L, FUH M R. Determination of phenylurea herbicides in aqueous samples using partitioned dispersive liquid-liquid microextration[J]. Talanta, 2009,80(2):493-498.
【12】陈园,张丽君,顾海东,等.分散固相萃取-UHPLC-MS/MS法测定水中5种苯脲类除草剂[J].化学试剂, 2016,38(3):245-248.
【13】HE Z Y, LIU D H, LI R H, et al. Magnetic solid-phase extration of sulfonylurea herbicides in environmental water samples by Fe3O4@dictadecyl dimethyl ammonium chloride@silica magnteic particles[J]. Analytica Chimica Acta, 2012,747:29-35.
【14】连丽丽,郭亭秀,吴玉清,等.磁性固相萃取-液相色谱法测定环境水样中痕量的微囊藻毒素[J].分析化学, 2015,43(12):1876-1881.
【15】白沙沙,李芝,臧晓欢,等.磁性石墨烯固相萃取-分散液液微萃取-气相色谱法测定水和绿茶中酰胺类除草剂残留[J].分析化学, 2013,41(8):1177-1182.
【16】张贵江,臧晓欢,周欣,等.磁性石墨烯纳米粒子固相萃取与气相色谱-质谱相结合测定环境水样中的三嗪类除草剂[J].色谱, 2013,31(11):1071-1075.
相关信息