QuEChERS-超高效液相色谱法快速测定果蔬中4种植物激素残留
|
摘要
目的建立超高效液相色谱法快速测定果蔬中4种植物激素残留方法。方法样品经甲醇提取后,提取液采用分散固相萃取吸附剂C_(18)进行吸附净化,用乙腈-0.02 mol/L乙酸铵溶液为流动相,Waters ACQUITY UPLC~?BEHC_(18)色谱柱分离进行液相色谱梯度洗脱,二极管阵列检测器200～400 nm检测,外标法定量。结果4种植物激素在0.1～4.0μg/mL范围内线性关系良好,相关系数r≥0.9997,其检出限为0.006～0.032 mg/kg,样品的加标回收率为83.8%～98.4%,相对标准偏差为2.06%～3.89%。结论该方法样品前处理简单,快速高效,重现性好,准确度高,适用于果蔬中4种植物激素残留的检测。
Objective To establish a rapid method for the determination of 4 kinds of phytohormone residues in fruits and vegetables by ultra performance liquid chromatography(UPLC). Methods After the sample was extracted with methanol, the extracted liquid was adsorbed and purified by dispersed solid phase extraction adsorbent C_(18). The mobile phase was acetonitrile-0.02 mol/L ammonium acetate solution. The sample was separated by Waters ACQUITY UPLC~?BEH C_(18) column for gradient elution, and was detected by diode array detector at 200～400 nm and quantified by external standard method. Results Four kinds of phytohormones had good linear relationships in the range of 0.1-4.0 μg/mL, and the correlation coefficients(r) was 0.9997. The limits of detection were 0.006～0.032 mg/kg. The average recoveries of 4 kinds of phytohormones were 83.8%-98.4%, with the relative standard deviations of 2.06%-3.89%. Conclusion This method is simple, rapid, efficient, reproducible and accurate, which is suitable for the detection of 4 kinds of plant hormones residues in fruits and vegetables.
Objective To establish a rapid method for the determination of 4 kinds of phytohormone residues in fruits and vegetables by ultra performance liquid chromatography(UPLC). Methods After the sample was extracted with methanol, the extracted liquid was adsorbed and purified by dispersed solid phase extraction adsorbent C_(18). The mobile phase was acetonitrile-0.02 mol/L ammonium acetate solution. The sample was separated by Waters ACQUITY UPLC~?BEH C_(18) column for gradient elution, and was detected by diode array detector at 200～400 nm and quantified by external standard method. Results Four kinds of phytohormones had good linear relationships in the range of 0.1-4.0 μg/mL, and the correlation coefficients(r) was 0.9997. The limits of detection were 0.006～0.032 mg/kg. The average recoveries of 4 kinds of phytohormones were 83.8%-98.4%, with the relative standard deviations of 2.06%-3.89%. Conclusion This method is simple, rapid, efficient, reproducible and accurate, which is suitable for the detection of 4 kinds of plant hormones residues in fruits and vegetables.
引文
[1]王文文,曹雪琴,杨中,等.植物生长调节剂在果树中的应用现状及残留分析方法研究进展[J].现代农业科技,2017,(12):129-131.Wang WW, Cao XQ, Yang Z,et al. Research advances on application status of plant growth regulators in fruit trees and its residue analysis[J].Mod Agric Sci Technol, 2017,(12):129-131.
[2]史晓梅,金芬,黄玉婷,等.水果中常用植物生长调节剂的研究进展[J].食品工业科技,2012, 33(4):417-422,426.Shi XM, Jin F, Huang YT, et al. Review on advance of plant growth regulators in fruits[J]. Food Ind Sci Technol, 2012,33(4):417-422, 426.
[3]GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[4]赵士权,查河霞,赵好.离子色谱法测定水果和蔬菜中2,4-二氯苯氧乙酸的含量[J].理化检验(化学分册),2016, 52(12):1435-1438.Zhao SQ, Zha HX, Zhao H. IC determination of 2,4-Dichlorophenoxyacetic acid in fruits and vegetables[J]. Phys Test Chem Anal B,2016, 52(12):1435-1438.
[5]王杏,周小倩,刘超,等.高效液相色谱法同时测定果蔬中6种植物激素的残留[J].食品安全质量检测学报,2018, 9(20):5376-5380.Wang X, Zhou XQ, Liu C, et al. Determination of 6 kinds of plant hormones residues in fruits and vegetables by high performance liquid chromatography[J]. J food Saf Qual, 2018, 9(20):5376-5380.
[6] Klinsunthorn N, Petsom A, Nhujak T. Determination of steroids adulterated in liquid herbal medicines using QuEChERS sample preparation and high performance liquid chromatography[J]. J PharmBiom Anal, 2011,55(5):1175-1178.
[7]朱群英,朱玉玲,索莉莉,等.在线固相萃取-高效液相色谱法同时测定豆芽中11种植物生长剂和杀菌剂[J].分析科学学报,2018, 34(4):507-512.Zhu QY, Zhu YL, Suo LL, et al. Simultaneous determination of eleven plant growth regulators and fungicides in bean sprouts by online solid phase extraction-high performance liquid chromatography[J]. J Anal Sci,2018, 34(4):507-512.
[8]朱松,袁晓晴,戴军,等.QuEChERS/HPLC/DAD法同时检测果蔬中多种植物激素残留[J].分析测试学报,2017, 36(4):513-518.Zhu S, Yuan XQ, Dai J, et al. Simultaneous determination of different phytohormones residues in fruits and vegetables by QuEChERS/DAD/HPLC[J]. J Instrum Anal, 2017, 36(4):513-518.
[9]马桂娟,汤丽华,朱捷,等.高效液相色谱串联质谱法测定豆芽中4种药物残留[J].食品研究与开发,2018,39(10):138-142.Ma GJ, Tang LH, Zhu J, et al. Determination of four drug residues in bean sprouts by high performance liquid chromatography-tandem mass spectrometry[J]. Food Res Dev, 2018, 39(10):138-142.
[10]张靖雯,郭春海,葛世辉,等.固相萃取-超高效液相色谱串联质谱法同时测定豆芽中6-苄基腺嘌呤、赤霉素和4-氯苯氧乙酸的残留量[J].中国食品卫生杂志,2014, 26(5):441-444.Zhang JW, Guo CH, Ge SH, et al. Simultaneous determination of6-benzylaminopurine, gibberellin and 4-chlorophenoxyacetic acid in bean sprouts by solid phase extractionultra high performance liquid chromatography tandem mass spectrometry[J]. Chin J Health Lab Technol,2014, 26(5):441-444.
[11]郭虹,任武洁,魏玉霞,等.分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜中7种植物生长调节剂[J].中国卫生检验杂志,2018,28(6):660-663, 666.Guo H, Rren WJ, Wei YX, et al. Determination of 7 kinds of plant growth regulators in vegetables by dispersive solid phase extraction ultra performance liquid chromatography tandem-mass spectrometry[J]. Chin J Health Lab Technol, 2018, 28(6):660-663, 666.
[12]周纯洁,赵博,吴丹,等.QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜中6种植物生长调节剂[J].食品工业科技,2016, 37(10):94-98, 10.Zhou CJ, Zhao B, Wu D, et al. Determination of six plant growth regulators in vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Ind Sci Technol,2016, 37(10):94-98, 10.
[13]薛荣旋,黄诚,刘国平,等.QuEChERS结合气相色谱-串联质谱法测定水果中5种植物生长调节剂[J].中国食品卫生杂志,2017, 29(5):561-566.Xue RX, Huang C, Liu GP, et al. Determination of five plant growth regulators in fruits by QuEChERS with gas chromatography-tandem mass spectrometry[J]. Chin J Health Lab Technol, 2017,29(5):561-566.
[14]刘印平,王丽英,路杨,等.河北省市售豆芽菜中6种植物生长调节剂残留调查分析[J].食品安全质量检测学报,2015,6(10):3827-3833.Liu YP, Wang LY, Lu Y, et al. Analysis of the residues of 6 kinds of plant growth regulators in bean sprouts in Hebei province[J]. J Food Saf Qual,2015,6(10):3827-3833.
[15]吴平谷,谭莹,张晶,等.分级净化结合气相色谱-质谱联用法测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.Wu PG, Tan Y, Zhang J, et al. Determination of 10 plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J]. Chin J Anal Chem, 2014,42(6):866-871.
[2]史晓梅,金芬,黄玉婷,等.水果中常用植物生长调节剂的研究进展[J].食品工业科技,2012, 33(4):417-422,426.Shi XM, Jin F, Huang YT, et al. Review on advance of plant growth regulators in fruits[J]. Food Ind Sci Technol, 2012,33(4):417-422, 426.
[3]GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].GB 2763-2016 National food safety standard-Maximum residue limits for pesticides in food[S].
[4]赵士权,查河霞,赵好.离子色谱法测定水果和蔬菜中2,4-二氯苯氧乙酸的含量[J].理化检验(化学分册),2016, 52(12):1435-1438.Zhao SQ, Zha HX, Zhao H. IC determination of 2,4-Dichlorophenoxyacetic acid in fruits and vegetables[J]. Phys Test Chem Anal B,2016, 52(12):1435-1438.
[5]王杏,周小倩,刘超,等.高效液相色谱法同时测定果蔬中6种植物激素的残留[J].食品安全质量检测学报,2018, 9(20):5376-5380.Wang X, Zhou XQ, Liu C, et al. Determination of 6 kinds of plant hormones residues in fruits and vegetables by high performance liquid chromatography[J]. J food Saf Qual, 2018, 9(20):5376-5380.
[6] Klinsunthorn N, Petsom A, Nhujak T. Determination of steroids adulterated in liquid herbal medicines using QuEChERS sample preparation and high performance liquid chromatography[J]. J PharmBiom Anal, 2011,55(5):1175-1178.
[7]朱群英,朱玉玲,索莉莉,等.在线固相萃取-高效液相色谱法同时测定豆芽中11种植物生长剂和杀菌剂[J].分析科学学报,2018, 34(4):507-512.Zhu QY, Zhu YL, Suo LL, et al. Simultaneous determination of eleven plant growth regulators and fungicides in bean sprouts by online solid phase extraction-high performance liquid chromatography[J]. J Anal Sci,2018, 34(4):507-512.
[8]朱松,袁晓晴,戴军,等.QuEChERS/HPLC/DAD法同时检测果蔬中多种植物激素残留[J].分析测试学报,2017, 36(4):513-518.Zhu S, Yuan XQ, Dai J, et al. Simultaneous determination of different phytohormones residues in fruits and vegetables by QuEChERS/DAD/HPLC[J]. J Instrum Anal, 2017, 36(4):513-518.
[9]马桂娟,汤丽华,朱捷,等.高效液相色谱串联质谱法测定豆芽中4种药物残留[J].食品研究与开发,2018,39(10):138-142.Ma GJ, Tang LH, Zhu J, et al. Determination of four drug residues in bean sprouts by high performance liquid chromatography-tandem mass spectrometry[J]. Food Res Dev, 2018, 39(10):138-142.
[10]张靖雯,郭春海,葛世辉,等.固相萃取-超高效液相色谱串联质谱法同时测定豆芽中6-苄基腺嘌呤、赤霉素和4-氯苯氧乙酸的残留量[J].中国食品卫生杂志,2014, 26(5):441-444.Zhang JW, Guo CH, Ge SH, et al. Simultaneous determination of6-benzylaminopurine, gibberellin and 4-chlorophenoxyacetic acid in bean sprouts by solid phase extractionultra high performance liquid chromatography tandem mass spectrometry[J]. Chin J Health Lab Technol,2014, 26(5):441-444.
[11]郭虹,任武洁,魏玉霞,等.分散固相萃取-超高效液相色谱-串联质谱法测定蔬菜中7种植物生长调节剂[J].中国卫生检验杂志,2018,28(6):660-663, 666.Guo H, Rren WJ, Wei YX, et al. Determination of 7 kinds of plant growth regulators in vegetables by dispersive solid phase extraction ultra performance liquid chromatography tandem-mass spectrometry[J]. Chin J Health Lab Technol, 2018, 28(6):660-663, 666.
[12]周纯洁,赵博,吴丹,等.QuEChERS-超高效液相色谱-串联质谱法同时测定蔬菜中6种植物生长调节剂[J].食品工业科技,2016, 37(10):94-98, 10.Zhou CJ, Zhao B, Wu D, et al. Determination of six plant growth regulators in vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Ind Sci Technol,2016, 37(10):94-98, 10.
[13]薛荣旋,黄诚,刘国平,等.QuEChERS结合气相色谱-串联质谱法测定水果中5种植物生长调节剂[J].中国食品卫生杂志,2017, 29(5):561-566.Xue RX, Huang C, Liu GP, et al. Determination of five plant growth regulators in fruits by QuEChERS with gas chromatography-tandem mass spectrometry[J]. Chin J Health Lab Technol, 2017,29(5):561-566.
[14]刘印平,王丽英,路杨,等.河北省市售豆芽菜中6种植物生长调节剂残留调查分析[J].食品安全质量检测学报,2015,6(10):3827-3833.Liu YP, Wang LY, Lu Y, et al. Analysis of the residues of 6 kinds of plant growth regulators in bean sprouts in Hebei province[J]. J Food Saf Qual,2015,6(10):3827-3833.
[15]吴平谷,谭莹,张晶,等.分级净化结合气相色谱-质谱联用法测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.Wu PG, Tan Y, Zhang J, et al. Determination of 10 plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J]. Chin J Anal Chem, 2014,42(6):866-871.