Simultaneous SPE-HPLC Determination of Residual Amounts of Plant Growth Regulators and Fungicides in Drink
摘 要
提出了高效液相色谱法同时测定饮料中2种植物生长调节剂(多菌灵、6-苄基腺嘌呤)和2种杀菌剂(多效唑、腈菌唑)含量。样品滤液过GDX501固相萃取小柱,经水-甲醇(80+20)混合溶液淋洗后,用甲醇洗脱。洗脱液在Waters Symmetry C18色谱柱上进行分离,流动相为甲醇与pH 6的5 mmol·L-1磷酸盐缓冲溶液(67+33)混合液。4种化合物的线性范围均为1.0~50 mg·L-1,检出限(3S/N)分别为0.24,0.80,0.90,0.90 mg·L-1。方法用于橙汁样品分析,回收率在70.9%~104%之间,相对标准偏差(n=6)均小于6%。
Abstract
A method for the simultaneous determination of 2 plant-growth regulators (carbendazim and 6-benzylaminopurine) and 2 fungicides (paclobutrazol and myclobutanil) in drinks by HPLC was proposed. The filtrate of sample was purified on GDX501 SPE column. The column was first rinsed with a mixed solution of H2O+CH3OH (80+20) and then eluted with CH3OH. The 4 compounds mentioned above were separated on Waters Symmetry C18 column with mixture of methanol and 5 mmol·L-1 phosphate buffer of pH 6 (67+33) as mobile phase. Linearity ranges for the 4 compounds were same between 1.0 and 50 mg·L-1, with detection limits (3S/N) of 0.24 (for carbendazim), 0.80 (for benzylaminopurine), 0.90 (for paclobutrazol) and 0.90 mg·L-1 (for myclobutanil). Sample of orange juice was analyzed by the proposed method, giving values of recovery in the range of 70.9%-104%, with RSD′s (n=6) less than 6%.
中图分类号 O652.63
所属栏目 工作简报
基金项目 浙江省自然科学基金资助项目(M203030,Y4110536);浙江省公益性技术应用研究(分析测试)项目(2011C37040)
收稿日期 2012/8/3
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备注张旭(1987-),女,浙江德清人,硕士,研究方向为色谱分析。
引用该论文: ZHANG Xu,WANG Guo-qing,YU Xiao-feng,WANG Li-li,PAN Zai-fa. Simultaneous SPE-HPLC Determination of Residual Amounts of Plant Growth Regulators and Fungicides in Drink[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(5): 559~562
张旭,王国琴,余晓峰,王丽丽,潘再法. 固相萃取-高效液相色谱法同时测定饮料中植物生长调节剂和杀菌剂残留量[J]. 理化检验-化学分册, 2013, 49(5): 559~562
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参考文献
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【2】轩梅.植物生长调节剂在甘薯生产上的应用[J].农村使用技术, 2008(2):49-49.
【3】白桦,邱月明,张青.气相色谱-质谱法测定苹果中多效唑残留量[J].分析测试学报, 2005,24(4):64-66.
【4】吴凤琪,靳保辉,陈波,等.水果中8种外源性植物生长调节剂的液相色谱-串联质谱测定[J].中国农学通报, 2010,26(15):115-119.
【5】杨安中,黄义德.旱作水稻喷施6-苄基腺嘌呤的防早衰及增产效应[J].南京农业大学学报, 2001,24(2):12-15.
【6】CURRY E A, WILLIAMS M W. Effect of paclobutrazol on fruit quality: apple, pear and cherry[J]. V International Symposium on Growth Regulators in Fruit Production, 1986,179:743-754.
【7】江培胜,沈言根,张家喜.40%多菌灵·三唑酮可湿性粉剂防治小麦主要病害应用技术研究[J].现代农业科技, 2007(18):69-70.
【8】楼正云,汤富彬,罗逢健,等.腈菌唑在黄瓜和土壤中的残留动态[J].农药, 2008,47(3):205-207.
【9】金米聪,陈晓红,李小平,等.HPLC/APCI/MS法测定水果中6-苄基腺嘌呤[J].分析仪器, 2005(3):29-31.
【10】SANCHO J V, POZO O J, ZAMORA T, et al. Direct determinstion of paclobutrazol residues in pear samples by liquid chromatography-electrospray tandem mass spectrometry[J]. J Agr Food Chem, 2003,51(15):4202-4206.
【11】蔡世炎,游文玮,李耀群.导数同步荧光法快速检测香菇中的多菌灵[J].分析测试学报, 2007,26(1):117-119.
【12】徐华能.蔬菜水果中腈菌唑农药残留气相色谱(ECD)检测法[J].农药, 2008,47(5):359-360.
【13】SUN Dong, ZHANG Hua-jie. Voltammetric determination of 6-benzylaminopurine (6-BA) using an acetylene black-dihexadecyl hydrogen phosphate composite film coated glassy carbon electrode[J]. J Chromatogr A, 2006,557(1/2):64-69.
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