液相色谱-串联质谱法同时测定浆果类、瓜果类水果中19种植物生长调节剂的残留量
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摘要
建立液相色谱-三重四级杆串联质谱法同时测定浆果类、瓜果类水果中19种植物生长调节剂残留量的检测方法。样品经优化的QuEChERS法进行前处理,用含1%乙酸的乙腈溶液提取,分散固相萃取净化,用Waters Acquity HSS T3色谱柱,乙腈和0.1%甲酸水溶液作为流动相进行梯度洗脱,采用电喷雾多反应监测模式,基质匹配标准溶液外标法定量。结果表明:19种植物生长调节剂在相应浓度范围内线性良好(r> 0.9902),该方法的检出限为0.09～16.8μg/kg,定量限为0.27～50.4μg/kg,加标回收率为69.4%～106.2%,RSD为1.1%～12.5%。随机检测200份样品,生长调节剂的检出率为6.3%。该方法灵敏度高,定性、定量准确,易于在实验室推广应用,可用于浆果类、瓜果类水果中的专属生长调节剂的测定。
To establish a method for the simultaneous determination of 19 plant growth regulators in berries and melons by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Samples were pretreated by the quick,easy,cheap,effective,rugged and safe (QuEChERS) improved method.The plant growth regulator residues were extracted from the samples by acetonitrile (containing 1% acetic acid),cleaned up with QuEChERS and then analyzed using HPLC-MS/MS in multiple reaction monitoring (MRM) mode.The chromatographic analysis was carried out on a Waters Acquity HSS T3 column with acetonitrile and 0.1% formic acid solution as the mobile phases in gradient program,and quantified by matrix-matched external standard method.The results showed that,19 kinds of plant growth regulators showed good linearity when they were in their concentration ranges (r > 0.9902).The limits of detection were within 0.09～16.8 μg/kg and the limits of quantification of the 19 plant growth regulators were within 0.27～50.4 μg/kg.The recoveries of 19 kinds of plant growth regulators were within 69.4% ～106.2%,RSD was 1.1% ～12.5%.Conclusion: The method was highly sensitive,qualitative and quantitative,easy to be used in the laboratory.It could be used to determine the specific growth regulators in berries and melons.
To establish a method for the simultaneous determination of 19 plant growth regulators in berries and melons by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS).Samples were pretreated by the quick,easy,cheap,effective,rugged and safe (QuEChERS) improved method.The plant growth regulator residues were extracted from the samples by acetonitrile (containing 1% acetic acid),cleaned up with QuEChERS and then analyzed using HPLC-MS/MS in multiple reaction monitoring (MRM) mode.The chromatographic analysis was carried out on a Waters Acquity HSS T3 column with acetonitrile and 0.1% formic acid solution as the mobile phases in gradient program,and quantified by matrix-matched external standard method.The results showed that,19 kinds of plant growth regulators showed good linearity when they were in their concentration ranges (r > 0.9902).The limits of detection were within 0.09～16.8 μg/kg and the limits of quantification of the 19 plant growth regulators were within 0.27～50.4 μg/kg.The recoveries of 19 kinds of plant growth regulators were within 69.4% ～106.2%,RSD was 1.1% ～12.5%.Conclusion: The method was highly sensitive,qualitative and quantitative,easy to be used in the laboratory.It could be used to determine the specific growth regulators in berries and melons.
引文
[1]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.
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[3]陈卫军,张耀海,李云成等.果蔬中常用植物生长调节剂分析方法研究进展[J].食品科学,2012,33(11):283-289.
[4]吴平谷,谭莹,张晶等.分级净化结合气相色谱-质谱联用发测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.
[5]Shi Xiao mei,Jin Fen,Huang Yuting,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(Qu ECh ERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural and Food Chemistry,2012,60(1):60-65.
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[9]刘柏林,谢继安,赵紫微等.稳定同位素内标/超高压液相色谱-串联质谱法同时测定水果与豆芽中10种植物生长调节剂残留[J].分析测试学报,2017,36(5):601-606.
[10]Guoliang Li,Shucheng Liu,Zhiwei Sun,et al.A simple and sensitive HPLC method based on pre-column fluorescence labelling for multiple classes of plant growth regulator determination in food samples[J].Food Chemistry,2015,170(1/3):123-130.
[11]Nadeem Muhammad,Qamar Subhani,Fenglian Wang,et al.Simultaneous determination of two plant growth regulators in ten food samples using ion chromatography combined with Qu ECh ERSextraction method(IC-Qu ECh ERS)and coupled with fluorescence detector[J].Food Chemistry,2018,241(15/2):308-316.
[12]Qian Lu,Jian-Hong Wu,Qiong-Wei Yu,et al.Using pollen grains as novel hydrophilic solid-phase extraction sorbents for the simultaneous determination of 16 plant growth regulators[J].Journal of Chromatography A,2014,1367(7/11):39-47.
[13]Hamaguchi T,Katsumata M,Nakano E,et al.Simultaneous determination of different endogenetic plant growth regulators in common green seaweeds using dispersive liquid-liquid microextraction method[J].Plant Physiology&Biochemistry,2011,49(11):1259-1263.
[14]Zhen Yan,Ji-Yun Nie,Yang Cheng,et al.Simultaneous determination of plant growth regulators in fruit by ultraperformance liquid chromatography-tandem mass spectrometry coupled with modified Qu ECh ERS procedure[J].Chinese Journal of Analytical Chemistry,2017,45(5/5):1719-1725.
[15]胡晓科,文君,邹海民等.高效液相色谱法同时测定蔬菜中10种植物生长调节剂残留[J].中国卫生检验杂志,2017,27(22):3218-3220.
[16]赵佳丽,徐盼盼,陈娟娟等.基于HPLC-Qq Q-MS/MS技术的坛紫菜中植物激素分析[J].食品科学,2016,37(16):216-222.
[17]程盛华,杨春亮,曾绍东等.分散固相萃取-超高效液相色谱-串质谱法测定豆芽中10种植物生长剂和杀菌剂[J].食品工业科技,2016,12(2):53-59.
[18]张泸文,焦广睿,王珂等.QuEChERS-高效液相色谱-串联质谱法同时测定果蔬中26种植物生长调节剂残留[J].食品安全质量检测学报,2016,7(7):2678-2687.
[2]王岚,林海丹,徐娟等.国内外植物生长调节剂残留限量标准的比对分析[J].广东农业科学,2015,42(3):70-73.
[3]陈卫军,张耀海,李云成等.果蔬中常用植物生长调节剂分析方法研究进展[J].食品科学,2012,33(11):283-289.
[4]吴平谷,谭莹,张晶等.分级净化结合气相色谱-质谱联用发测定豆芽中10种植物生长调节剂[J].分析化学,2014,42(6):866-871.
[5]Shi Xiao mei,Jin Fen,Huang Yuting,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(Qu ECh ERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural and Food Chemistry,2012,60(1):60-65.
[6]Xuejin Mao,Lijuan Tang,Ting Tan,et al.Determination o plant growth regulators in pears by microwave-assisted extraction and liquid chromatography with electrospray ionization mass spectrometry[J].Journal of Separation Science,2014,37(11):1352-1358.
[7]Lehotay S J,Son K A,Kwon H,et al.Comparison o Qu ECh ERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1217:2548-2560.
[8]Cho S,El-Aty A,Park K,et al.Simple multi-residue extraction method for the determination of fungicides and plant growth regulator in bean sprouts using low temperature partitioning and tandem mass spectrometry[J].Food Chemistry,2013,136(3/4):1414-1420.
[9]刘柏林,谢继安,赵紫微等.稳定同位素内标/超高压液相色谱-串联质谱法同时测定水果与豆芽中10种植物生长调节剂残留[J].分析测试学报,2017,36(5):601-606.
[10]Guoliang Li,Shucheng Liu,Zhiwei Sun,et al.A simple and sensitive HPLC method based on pre-column fluorescence labelling for multiple classes of plant growth regulator determination in food samples[J].Food Chemistry,2015,170(1/3):123-130.
[11]Nadeem Muhammad,Qamar Subhani,Fenglian Wang,et al.Simultaneous determination of two plant growth regulators in ten food samples using ion chromatography combined with Qu ECh ERSextraction method(IC-Qu ECh ERS)and coupled with fluorescence detector[J].Food Chemistry,2018,241(15/2):308-316.
[12]Qian Lu,Jian-Hong Wu,Qiong-Wei Yu,et al.Using pollen grains as novel hydrophilic solid-phase extraction sorbents for the simultaneous determination of 16 plant growth regulators[J].Journal of Chromatography A,2014,1367(7/11):39-47.
[13]Hamaguchi T,Katsumata M,Nakano E,et al.Simultaneous determination of different endogenetic plant growth regulators in common green seaweeds using dispersive liquid-liquid microextraction method[J].Plant Physiology&Biochemistry,2011,49(11):1259-1263.
[14]Zhen Yan,Ji-Yun Nie,Yang Cheng,et al.Simultaneous determination of plant growth regulators in fruit by ultraperformance liquid chromatography-tandem mass spectrometry coupled with modified Qu ECh ERS procedure[J].Chinese Journal of Analytical Chemistry,2017,45(5/5):1719-1725.
[15]胡晓科,文君,邹海民等.高效液相色谱法同时测定蔬菜中10种植物生长调节剂残留[J].中国卫生检验杂志,2017,27(22):3218-3220.
[16]赵佳丽,徐盼盼,陈娟娟等.基于HPLC-Qq Q-MS/MS技术的坛紫菜中植物激素分析[J].食品科学,2016,37(16):216-222.
[17]程盛华,杨春亮,曾绍东等.分散固相萃取-超高效液相色谱-串质谱法测定豆芽中10种植物生长剂和杀菌剂[J].食品工业科技,2016,12(2):53-59.
[18]张泸文,焦广睿,王珂等.QuEChERS-高效液相色谱-串联质谱法同时测定果蔬中26种植物生长调节剂残留[J].食品安全质量检测学报,2016,7(7):2678-2687.