QuEChERS-高效液相色谱法测定铁皮石斛中多菌灵和甲基硫菌灵的残留量
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摘要
目的:建立QuEChERS-高效液相色谱法测定不同产地铁皮石斛中多菌灵与甲基硫菌灵农药残留量的方法。方法:铁皮石斛样品用乙腈溶液提取,经QuEChERS方法净化,采用Waters C_(18)色谱柱(150 mm×4.6mm,5μm)、乙腈-0.02 mol/L乙酸铵缓冲溶液(20∶80)为流动相,流速1 mL/min、柱温35℃、检测波长280 nm,对不同产地铁皮石斛中多菌灵与甲基硫菌灵残留量进行检测。结果:多菌灵在0.05~25 mg/L范围内呈良好的线性关系,相关系数等于0.999 4,检测限为0.01 mg/kg,定量限为0.04 mg/kg,3个添加水平下的平均回收率是98.28%,RSD是2.68%;甲基硫菌灵在0.025~12.5 mg/L范围内呈良好的线性关系,相关系数等于0.999 5,检测限为0.02 mg/kg,定量限为0.06 mg/kg,3个添加水平下的平均回收率是101.03%,RSD是3.64%;50批铁皮石斛中有4批分别检出多菌灵与甲基硫菌灵农药残留,均低于《中国药典》2015年版中药有害残留物限量制定指导原则农药残留量最大限量理论值。结论:建立的QuEChERS-高效液相色谱法检测多菌灵和甲基硫菌灵,具有操作简单,高效、专属性好、重复性强、结果准确可靠等优点。
Objective: To establish a method for simultaneous determination of residual carbendazim and thiophanate-methyl in Dendrobium officinale from different regions by QuEChERS-HPLC. Methods: The samples were extracted by acetonitrile and purified by the optimized QuEChERS method.Then the carbendazim and thiophanate-methyl residues in Dendrobium officinale from different regions were determined by HPLC method with Waters C18 column( 150 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile-0. 02 mol/L ammonium acetate buffer for isogradient elution( 20∶ 80). The flow rate was 1 m L·min-1. The column temperature was 35 ℃ and the detection wavelength was 280 nm.Results: When the concentrations ranged from 0. 05 to 25 mg/L,the linear relationship was good( r =0. 999 4) in the case of with carbendazim. The detection limit was 0. 01 mg/kg,the quantitative limit was 0. 04 mg/kg,and the average recovery and RSD under three different levels of addition were98. 28% and 2. 68%; When the concentrations ranged from 0. 025 to 12. 5 mg/L,the linear relationship was also good( r = 0. 999 5) in the case with thiophanate-methyl. The detection limit was 0. 02 mg/kg,the quantitative limits was 0. 06 mg/kg,and the average recovery and RSD under three different levels of addition were 101. 03% and 3. 64%. The residue of carbendazim and thiophanate-methyl were detected in 4 batches among 50 batches of Dendrobium officinale,but lower than the theoretical value of maximum limit of pesticide residue in the guideline for the limitation of harmful residues of traditional Chinese medicine from China Pharmacopeia( 2015 edition). Conclusion: The Qu ECh ERHPLC method was established for the determination of carbendazim and thiophanate-methyl in the Dendrobium officinale. This method is simple and efficient with good specificity and strong repeatability.The results are accurate and reliable,providing real and effective basis for the quality control of Dendrobium candidum.
Objective: To establish a method for simultaneous determination of residual carbendazim and thiophanate-methyl in Dendrobium officinale from different regions by QuEChERS-HPLC. Methods: The samples were extracted by acetonitrile and purified by the optimized QuEChERS method.Then the carbendazim and thiophanate-methyl residues in Dendrobium officinale from different regions were determined by HPLC method with Waters C18 column( 150 mm × 4. 6 mm,5 μm). The mobile phase was acetonitrile-0. 02 mol/L ammonium acetate buffer for isogradient elution( 20∶ 80). The flow rate was 1 m L·min-1. The column temperature was 35 ℃ and the detection wavelength was 280 nm.Results: When the concentrations ranged from 0. 05 to 25 mg/L,the linear relationship was good( r =0. 999 4) in the case of with carbendazim. The detection limit was 0. 01 mg/kg,the quantitative limit was 0. 04 mg/kg,and the average recovery and RSD under three different levels of addition were98. 28% and 2. 68%; When the concentrations ranged from 0. 025 to 12. 5 mg/L,the linear relationship was also good( r = 0. 999 5) in the case with thiophanate-methyl. The detection limit was 0. 02 mg/kg,the quantitative limits was 0. 06 mg/kg,and the average recovery and RSD under three different levels of addition were 101. 03% and 3. 64%. The residue of carbendazim and thiophanate-methyl were detected in 4 batches among 50 batches of Dendrobium officinale,but lower than the theoretical value of maximum limit of pesticide residue in the guideline for the limitation of harmful residues of traditional Chinese medicine from China Pharmacopeia( 2015 edition). Conclusion: The Qu ECh ERHPLC method was established for the determination of carbendazim and thiophanate-methyl in the Dendrobium officinale. This method is simple and efficient with good specificity and strong repeatability.The results are accurate and reliable,providing real and effective basis for the quality control of Dendrobium candidum.
引文
[1]孙恒,胡强,金航,等.铁皮石斛化学成分及药理活性研究进展[J].中国实验方剂学杂志,2017,23(11):225-234.
[2]杨传玉,刘帆,吴耽,等.铁皮石斛抗阿司匹林诱导急性胃黏膜损伤活性组分筛选及作用研究[J].天然产物研究与开发,2016,28(11):1699-1705.
[3]吴耽,江婷婷,赵青,等.铁皮石斛多糖抗阿司匹林诱导人胃黏膜上皮细胞GES-1损伤的保护作用机制研究[J].中国药理学通报,2017,33(10):1479-1480.
[4]李戈,李荣英,高微微.药用石斛规模化种植中的病害问题及防治策略[J].中国中药杂志,2013,38(4):485-488
[5]戴燕萍.铁皮石斛生产质量管理规范研究[D].浙江农林大学,2012.
[6]吴永江,朱炜,程翼宇.液-质联用法测定铁皮石斛和西洋参及制剂中多菌灵残留[J].分析化学,2006,34(2):235-238.
[7]吴浪,张勇,李存雄,等.HPLC法测定苦荞中多菌灵的残留量[J].江西师范大学学报:自然科学版,2015,39(3):246-248.
[8]沈菁,刘军,刘建.高效液相色谱法测定柑橘和土壤中残留的多菌灵[J].色谱,2009,27(3):308-312.
[9]高国文,刘育清,朱家香.液相色谱法检测柑橘中多菌灵残留的方法研究[J].农药科学与管理,2006,27(5):10-11.
[10]刘静,李明.高效液相色谱法测定水稻及土壤中甲基硫菌灵和多菌灵[J].湖北农业科学,2013,52(5):1151-1153.
[11]周雪晴,谢艳丽,张青,等.高效液相色谱法测定香蕉中的多菌灵、噻菌灵、甲基硫菌灵[J].化学分析计量,2012,21(2):34-36.
[12]刘杰,杨春亮,查玉兵,等.高效液相色谱法-荧光检测器同时检测龙眼中多菌灵和噻菌灵残留[J].广东农业科学,2010,37(3):150-152.
[13]张念洁,吴信子,姜旭.高效液相色谱法同时测定人参中多菌灵和甲基硫菌灵农药残留的含量[J].现代食品科技,2013,29(4):907-910.
[14]朱军,陈琴华,李鹏,等.LC-MS/MS法测定金银花中多菌灵的残留量[J].中国药师,2016,19(4):664-666.
[15]张志勇,龚勇,单炜力,等.Qu ECh ERS-高效液相色谱-串联质谱法测定黄瓜和土壤中甲基硫菌灵和多菌灵[J].色谱,2012,30(1):91-94.
[16]赵连海,于淑新,孙元社,等.Qu ECh ERS-高效液相色谱法测定果蔬中多菌灵残留[J].农业工程,2012,2(7):42-44.
[2]杨传玉,刘帆,吴耽,等.铁皮石斛抗阿司匹林诱导急性胃黏膜损伤活性组分筛选及作用研究[J].天然产物研究与开发,2016,28(11):1699-1705.
[3]吴耽,江婷婷,赵青,等.铁皮石斛多糖抗阿司匹林诱导人胃黏膜上皮细胞GES-1损伤的保护作用机制研究[J].中国药理学通报,2017,33(10):1479-1480.
[4]李戈,李荣英,高微微.药用石斛规模化种植中的病害问题及防治策略[J].中国中药杂志,2013,38(4):485-488
[5]戴燕萍.铁皮石斛生产质量管理规范研究[D].浙江农林大学,2012.
[6]吴永江,朱炜,程翼宇.液-质联用法测定铁皮石斛和西洋参及制剂中多菌灵残留[J].分析化学,2006,34(2):235-238.
[7]吴浪,张勇,李存雄,等.HPLC法测定苦荞中多菌灵的残留量[J].江西师范大学学报:自然科学版,2015,39(3):246-248.
[8]沈菁,刘军,刘建.高效液相色谱法测定柑橘和土壤中残留的多菌灵[J].色谱,2009,27(3):308-312.
[9]高国文,刘育清,朱家香.液相色谱法检测柑橘中多菌灵残留的方法研究[J].农药科学与管理,2006,27(5):10-11.
[10]刘静,李明.高效液相色谱法测定水稻及土壤中甲基硫菌灵和多菌灵[J].湖北农业科学,2013,52(5):1151-1153.
[11]周雪晴,谢艳丽,张青,等.高效液相色谱法测定香蕉中的多菌灵、噻菌灵、甲基硫菌灵[J].化学分析计量,2012,21(2):34-36.
[12]刘杰,杨春亮,查玉兵,等.高效液相色谱法-荧光检测器同时检测龙眼中多菌灵和噻菌灵残留[J].广东农业科学,2010,37(3):150-152.
[13]张念洁,吴信子,姜旭.高效液相色谱法同时测定人参中多菌灵和甲基硫菌灵农药残留的含量[J].现代食品科技,2013,29(4):907-910.
[14]朱军,陈琴华,李鹏,等.LC-MS/MS法测定金银花中多菌灵的残留量[J].中国药师,2016,19(4):664-666.
[15]张志勇,龚勇,单炜力,等.Qu ECh ERS-高效液相色谱-串联质谱法测定黄瓜和土壤中甲基硫菌灵和多菌灵[J].色谱,2012,30(1):91-94.
[16]赵连海,于淑新,孙元社,等.Qu ECh ERS-高效液相色谱法测定果蔬中多菌灵残留[J].农业工程,2012,2(7):42-44.
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