超高效液相色谱串联质谱测定蔬菜中23种植物生长调节剂残留
|
摘要
通过前处理及仪器条件优化,建立蔬菜中玉米素、芸薹素内酯、5-硝基愈创木酚钠等23种植物生长调节剂的QuEChERS-超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测方法。样品经φ=1%甲酸-乙腈溶液提取,硅藻土、C18净化,T3柱分离,电喷雾技术(ESI)和多反映监测模式(MRM)进行检测。结果表明,蔬菜中23种植物生长调节剂的平均加标回收率为73.1%～121.3%,检出限为0.007 1～4.3μg·kg~(-1),定量限为0.024～14μg·kg~(-1)。所建立的方法简单、快速、有效,能够同时测定蔬菜中性质相差较大的23种植物生长调节剂,极大地节约了分析时间和成本。
The aim of this study is to develop a simple,fast and effective method for simultaneously determination 23 types of plant growth regulators(PGRs)in vegetables.The pretreatment by using QuEChERs for different PGRs and UPLC-MS/MS analysis were optimized.Samples were extracted by acetonitril with 1%acetic acid,purifed by high strength silica(HSS)HPLC columns filled with diatomite,C18.The determination of mass spectrometry was separated by T3 chromatographic column and achieved by electron spray ionization(ESI)and multiple reaction monitoring(MRM).The results indicated that the average spiked recoveries of 23 types of plant growth regulators(PGRs)in vegetables were 73.1%-121.3%,the LODs were 0.007 1-4.3μg·kg~(-1),and the LOQs were 0.024-14μg·kg~(-1).The method was rapid and simple with high sensitivity and good reproducibility,and suitable for the determination of 23 types of plant growth regulators(PGRs)in vegetables,so the analysis time and cost are greatly saved.
The aim of this study is to develop a simple,fast and effective method for simultaneously determination 23 types of plant growth regulators(PGRs)in vegetables.The pretreatment by using QuEChERs for different PGRs and UPLC-MS/MS analysis were optimized.Samples were extracted by acetonitril with 1%acetic acid,purifed by high strength silica(HSS)HPLC columns filled with diatomite,C18.The determination of mass spectrometry was separated by T3 chromatographic column and achieved by electron spray ionization(ESI)and multiple reaction monitoring(MRM).The results indicated that the average spiked recoveries of 23 types of plant growth regulators(PGRs)in vegetables were 73.1%-121.3%,the LODs were 0.007 1-4.3μg·kg~(-1),and the LOQs were 0.024-14μg·kg~(-1).The method was rapid and simple with high sensitivity and good reproducibility,and suitable for the determination of 23 types of plant growth regulators(PGRs)in vegetables,so the analysis time and cost are greatly saved.
引文
[1]谢文,史颖珠,侯建波,等.液相色谱-串联质谱法同时测定棉花中乙烯利、噻苯隆和敌草隆药物的残留量[J].色谱,2014,32(2):179-183.XIE W,SHI Y ZH,HOU J B,et al.Simultaneous determination of ethephon,thidiazuron,diuron residues in cotton by using high perfbrmance liquid chromatography-tandem mass spectrometry[J].Chinese Jouranl of Chromatography,2014,32(2):179-183.
[2]牟艳莉,郭德华,丁卓平,等.高效液相色谱·串联质谱法测定瓜果中11种植物生长调节剂的残留量[J].分析化学,2013,41(11):1640-1646.MOU Y L,GUO D H,DING ZH P,et al.Determination of11kinds of plant growth regulator residues in fruits and melons by high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2013,41(11):1640-1646.
[3]黄何何,张缙,徐敦明,等.QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J].色谱,2014,32(7):707-716.HUANG H H,ZHANG J,XU D M,et al.Determination of21plant growth regulator residues in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J].Chinese Jouranl of Chromatography,2014,32(7):707-716.
[4]栗有志,李艳美,尚爽,等.QuEChERS/液相色谱-串联质谱法测定果蔬中乙烯利残留[J].分析测试学报,2013,32(10):1237-1241.SU Y ZH,LI Y M,SHANG SH,et al.Determination of ethephon residue in fruits and vegetables by QuEChERS/high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis,2013,32(10):1237-1241.
[5]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):2678-2689.ZHANG L W,JIAO G R,WANG K,et al.Simultaneous determination of 26kinds of plant growth regulator residues in fruits and vegetable by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety and Quality,2016,7(7):2678-2689.
[6]诸力,王晨,陈红平.等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.ZHU L,WANG CH,CHEN H P,et al.Simultaneous determination of plant growth regulators and imidacloprid,acetamiprid in tea by ultra performance liquid chromatographytandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(4):529-536.
[7]张维一,周颖,都林娜,等.基质固相分散-气质联用法快速检测黄瓜中4类农药残留[J].浙江农业学报,2015,27(6):1000-1007.ZHANG W Y,ZHOU Y,DU L N,et al.Simultaneous determination of four types of pesticide residues in cucumber by matrix solidphase dispersion-GC-MS[J].Acta Agriculturae Zhejiangensis,2015,27(6):1000-1007.
[8]张文华,谢文,侯建波,等.气相色谱-串联质谱法测定豆芽与番茄中6种植物生长调节剂[J].分析测试学报,2016,35(10):1241-1247.ZHANG W H,XIE W,HOU J B,et al.Determination of 6plant growth regulators in bean sprout and tomato by gas chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis,2016,35(10):1241-1247.
[9]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 P G,TAN Y,ZHANG J,et al.Determination of 10plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(6):866-871.
[10]邓正正,王力华,王庆礼,等.植物生长调节剂对水曲柳组培苗生长及内源激素的影响[J].东北林业大学学报,2009,37(12):10-13.DENG ZH ZH,WANG L H,WANG Q L,et al.Effects of plant growth regulators on growth and endogenous hormones of in vitro plantlets of manchurian[J].Journal of Northeast Forestry University,2009,37(12):10-13.
[11]梁秀美,王祥云,薛晓峰,等.液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物[J].分析化学,2017,45(4):553-559.LIANG X M,WANG X Y,XUE X F,et al.Determination of imidacloprid and its three metabolites in honey and bee pollen by liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(4):553-559.
[12]董亚蕾,刘文倩,曹进,等.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学,2017,45(9):1397-1404.DONG Y L,LIU W Q,CAO J,et al.Determination of 38kinds of pesticide residues in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(9):1397-1404.
[13]吴岩,赵伟,刘永,等.快速基质分散净化-超快速液相色谱-串联质谱法同时测定玉米中22种三嗪类除草剂残留[J].分析化学,2016,44(6):950-957.WU Y,ZHAO W,LIU Y,et al.Determination of 22triazine herbicides residual in corn by enhanced matrix removal QuEChERS-ultra flow liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2016,44(6):950-957.
[14]张宪臣,李蓉,周艳萍,等.QuEChERS-超高效液相色谱-串联质谱法测定食用菌中7种荧光增白剂[J].分析化学,2017,45(5):777-783.ZHANG X CH,LI R,ZHOU Y P,et al.Simultaneous determination of seven kinds of fluorescent white agents in mushroom by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(5):777-783.
[15]张爱芝,王全林,曹丽丽,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱,2016,34(2):158-164.ZHANG A ZH,WANG Q L,CAO L L,et al.Determination of 250pesticide residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2016,34(2):158-164.
[2]牟艳莉,郭德华,丁卓平,等.高效液相色谱·串联质谱法测定瓜果中11种植物生长调节剂的残留量[J].分析化学,2013,41(11):1640-1646.MOU Y L,GUO D H,DING ZH P,et al.Determination of11kinds of plant growth regulator residues in fruits and melons by high performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2013,41(11):1640-1646.
[3]黄何何,张缙,徐敦明,等.QuEChERS-高效液相色谱-串联质谱法同时测定水果中21种植物生长调节剂的残留量[J].色谱,2014,32(7):707-716.HUANG H H,ZHANG J,XU D M,et al.Determination of21plant growth regulator residues in fruits by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J].Chinese Jouranl of Chromatography,2014,32(7):707-716.
[4]栗有志,李艳美,尚爽,等.QuEChERS/液相色谱-串联质谱法测定果蔬中乙烯利残留[J].分析测试学报,2013,32(10):1237-1241.SU Y ZH,LI Y M,SHANG SH,et al.Determination of ethephon residue in fruits and vegetables by QuEChERS/high performance liquid chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis,2013,32(10):1237-1241.
[5]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):2678-2689.ZHANG L W,JIAO G R,WANG K,et al.Simultaneous determination of 26kinds of plant growth regulator residues in fruits and vegetable by QuEChERS-high performance liquid chromatography-tandem mass spectrometry[J].Journal of Food Safety and Quality,2016,7(7):2678-2689.
[6]诸力,王晨,陈红平.等.超高效液相色谱-串联质谱法同时测定茶叶中11种植物生长调节剂及吡虫啉、啶虫脒的残留[J].分析化学,2017,45(4):529-536.ZHU L,WANG CH,CHEN H P,et al.Simultaneous determination of plant growth regulators and imidacloprid,acetamiprid in tea by ultra performance liquid chromatographytandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(4):529-536.
[7]张维一,周颖,都林娜,等.基质固相分散-气质联用法快速检测黄瓜中4类农药残留[J].浙江农业学报,2015,27(6):1000-1007.ZHANG W Y,ZHOU Y,DU L N,et al.Simultaneous determination of four types of pesticide residues in cucumber by matrix solidphase dispersion-GC-MS[J].Acta Agriculturae Zhejiangensis,2015,27(6):1000-1007.
[8]张文华,谢文,侯建波,等.气相色谱-串联质谱法测定豆芽与番茄中6种植物生长调节剂[J].分析测试学报,2016,35(10):1241-1247.ZHANG W H,XIE W,HOU J B,et al.Determination of 6plant growth regulators in bean sprout and tomato by gas chromatography-tandem mass spectrometry[J].Journal of Instrumental Analysis,2016,35(10):1241-1247.
[9]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 P G,TAN Y,ZHANG J,et al.Determination of 10plant growth regulators in bean sprouts by sequential cleaning-gas chromatography-mass spectrometry[J].Chinese Journal of Analytical Chemistry,2014,42(6):866-871.
[10]邓正正,王力华,王庆礼,等.植物生长调节剂对水曲柳组培苗生长及内源激素的影响[J].东北林业大学学报,2009,37(12):10-13.DENG ZH ZH,WANG L H,WANG Q L,et al.Effects of plant growth regulators on growth and endogenous hormones of in vitro plantlets of manchurian[J].Journal of Northeast Forestry University,2009,37(12):10-13.
[11]梁秀美,王祥云,薛晓峰,等.液相色谱-串联质谱法测定蜂产品中吡虫啉及其3种代谢物[J].分析化学,2017,45(4):553-559.LIANG X M,WANG X Y,XUE X F,et al.Determination of imidacloprid and its three metabolites in honey and bee pollen by liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(4):553-559.
[12]董亚蕾,刘文倩,曹进,等.QuEChERS-超高效液相色谱-串联质谱法测定坚果中38种农药残留[J].分析化学,2017,45(9):1397-1404.DONG Y L,LIU W Q,CAO J,et al.Determination of 38kinds of pesticide residues in nuts by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(9):1397-1404.
[13]吴岩,赵伟,刘永,等.快速基质分散净化-超快速液相色谱-串联质谱法同时测定玉米中22种三嗪类除草剂残留[J].分析化学,2016,44(6):950-957.WU Y,ZHAO W,LIU Y,et al.Determination of 22triazine herbicides residual in corn by enhanced matrix removal QuEChERS-ultra flow liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2016,44(6):950-957.
[14]张宪臣,李蓉,周艳萍,等.QuEChERS-超高效液相色谱-串联质谱法测定食用菌中7种荧光增白剂[J].分析化学,2017,45(5):777-783.ZHANG X CH,LI R,ZHOU Y P,et al.Simultaneous determination of seven kinds of fluorescent white agents in mushroom by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Analytical Chemistry,2017,45(5):777-783.
[15]张爱芝,王全林,曹丽丽,等.QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱,2016,34(2):158-164.ZHANG A ZH,WANG Q L,CAO L L,et al.Determination of 250pesticide residues in vegetables using QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chinese Journal of Chromatography,2016,34(2):158-164.