固相萃取-超高效液相色谱-串联质谱法测定果蔬中34种植物生长调节剂的残留量
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摘要
提出了固相萃取-超高效液相色谱-串联质谱法同时测定果蔬中34种植物生长调节剂残留量的方法。样品2.000 0g用乙腈10.0mL提取,经Oasis PRiME HLB固相萃取柱净化。取流出液5.0mL,氮气吹至近干,用甲醇(1+9)溶液溶解残渣并定容至1.0mL。以Waters CSH氟苯基色谱柱为固定相,以甲醇-5mmol·L-1乙酸铵溶液[含0.10%(体积分数)乙酸]为流动相进行梯度洗脱,采用电喷雾正、负离子源和多反应监测模式检测,外标法定量。34种植物生长调节剂在一定范围内呈线性关系,检出限(3S/N)为0.01~0.20μg·kg-1。按标准加入法进行回收试验,回收率为71.0%~115%,测定值的相对标准偏差(n=6)为0.60%~16%。
A method was proposed for the simultaneous determination of residual amounts of 34 plant growth regulators in fruits and vegetables by UPLC-MS/MS with solid phase extraction.The sample of 2.000 0 g was extracted with 10.0 mL of acetonitrile and purified by passing through Oasis PRiME HLB solid phase extraction column.The eluate of 5.0 mL was taken and concentrated to dryness by N2-blowing,and the residue was dissolved and made its volume up to 1.0 mL with methanol(1+9)solution.The Waters CSH fluorophenyl chromatographic column was used as stationary phase,and the mixture of methanol and 5 mmol·L-1 ammonium acetate solution containing 0.1%(φ)acetic acid was used as mobile phase for gradient elution.ESI+,ESI-and the mode of multireaction monitoring were adopted in MS/MS,and external standard method was used for quantification.Linear relationships of 34 plant growth regulators were found in definite ranges,with detection limits(3 S/N)in the range of 0.01-0.20μg·kg-1.Test for recovery was made by standard addition method,giving results in the range of71.0%-115%,with RSDs(n=6)ranged from 0.60%to 16%.
A method was proposed for the simultaneous determination of residual amounts of 34 plant growth regulators in fruits and vegetables by UPLC-MS/MS with solid phase extraction.The sample of 2.000 0 g was extracted with 10.0 mL of acetonitrile and purified by passing through Oasis PRiME HLB solid phase extraction column.The eluate of 5.0 mL was taken and concentrated to dryness by N2-blowing,and the residue was dissolved and made its volume up to 1.0 mL with methanol(1+9)solution.The Waters CSH fluorophenyl chromatographic column was used as stationary phase,and the mixture of methanol and 5 mmol·L-1 ammonium acetate solution containing 0.1%(φ)acetic acid was used as mobile phase for gradient elution.ESI+,ESI-and the mode of multireaction monitoring were adopted in MS/MS,and external standard method was used for quantification.Linear relationships of 34 plant growth regulators were found in definite ranges,with detection limits(3 S/N)in the range of 0.01-0.20μg·kg-1.Test for recovery was made by standard addition method,giving results in the range of71.0%-115%,with RSDs(n=6)ranged from 0.60%to 16%.
引文
[1]郝杰,冯楠,姜洁,等.水果蔬菜中常见植物生长调节剂分析检测方法研究进展[J].食品科学,2015,36(21):303-309.
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[3]吴莉莉,吕媛媛,沈兵,等.高效液相色谱-串联质谱法快速测定水果中氯吡脲残留量[J].理化检验-化学分册,2014,50(2):206-209.
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[5]戴莹,王纪华,韩平,等.农产品中6种植物生长调节剂残留限量标准及检测方法研究进展[J].食品安全质量检测学报,2016,7(2):425-432.
[6]朱杰丽,杨柳,柴振林,等.国内外植物生长调节剂限量标准分析研究[J].生物灾害科学,2013,36(2):232-236.
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[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.
[10]JIANG X X,SHI H Y,WU N,et al.Development of an enzyme-linked immunosorbent assay for diniconazole in agricultural samples[J].Food Chemistry,2010,125(4):1385-1389.
[11]张玉芬,席海山,谢凤山,等.毛细管胶束电泳测定番茄中环境激素2,4-滴的含量[J].农药,2007,46(9):607-608.
[12]孙武勇,魏东伟,刘海芳,等.高效液相色谱法测定棉花中3种脱叶剂的残留量[J].理化检验-化学分册,2014,50(1):112-113.
[13]谢柳青,孟昭礼,江树人,等.气相色谱法测定土壤和小白菜中胺鲜酯残留量[J].分析试验室,2008,27(11):68-70.
[14]邱暑婷,林学飞,傅冰梦,等.QuEChERS/高效液相色谱-串联质谱法同时测定葡萄中18种植物生长调节剂残留[J].中国卫生检验杂志,2017,27(7):931-936.
[15]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.
[16]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.
[17]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.
[18]SHI X M,JIN F,HUANG Y T,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural and Food Chemistry,2012,60(1):60-65.
[19]YAN Z,NIE J Y,XU G F,et al.Simultaneous determination of plant growth regulators in fruits using a modified QuEChERS procedure and UPLC-MS/MS[J].Horticultural Plant Journal,2016,2(4):203-208.
[2]徐鹏.食品和水中氨基甲酸酯农药及植物激素的液相色谱分析[D].保定:河北大学,2012.
[3]吴莉莉,吕媛媛,沈兵,等.高效液相色谱-串联质谱法快速测定水果中氯吡脲残留量[J].理化检验-化学分册,2014,50(2):206-209.
[4]李娜,郭藤,刘学.高效液相色谱-串联质谱法测定农产品中矮壮素残留量[J].理化检验-化学分册,2015,51(3):336-339.
[5]戴莹,王纪华,韩平,等.农产品中6种植物生长调节剂残留限量标准及检测方法研究进展[J].食品安全质量检测学报,2016,7(2):425-432.
[6]朱杰丽,杨柳,柴振林,等.国内外植物生长调节剂限量标准分析研究[J].生物灾害科学,2013,36(2):232-236.
[7]吴翚,宛瑜.脱落酸(ABA)荧光性质的研究[J].徐州师范大学学报(自然科学版),2002,20(2):39-41.
[8]虞淼,吴淑春.高效液相色谱-串联质谱同时测定草莓、杨梅中20种植物生长调节剂残留[J].食品科学,2015,36(24):246-252.
[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.
[10]JIANG X X,SHI H Y,WU N,et al.Development of an enzyme-linked immunosorbent assay for diniconazole in agricultural samples[J].Food Chemistry,2010,125(4):1385-1389.
[11]张玉芬,席海山,谢凤山,等.毛细管胶束电泳测定番茄中环境激素2,4-滴的含量[J].农药,2007,46(9):607-608.
[12]孙武勇,魏东伟,刘海芳,等.高效液相色谱法测定棉花中3种脱叶剂的残留量[J].理化检验-化学分册,2014,50(1):112-113.
[13]谢柳青,孟昭礼,江树人,等.气相色谱法测定土壤和小白菜中胺鲜酯残留量[J].分析试验室,2008,27(11):68-70.
[14]邱暑婷,林学飞,傅冰梦,等.QuEChERS/高效液相色谱-串联质谱法同时测定葡萄中18种植物生长调节剂残留[J].中国卫生检验杂志,2017,27(7):931-936.
[15]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.
[16]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.
[17]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.
[18]SHI X M,JIN F,HUANG Y T,et al.Simultaneous determination of five plant growth regulators in fruits by modified quick,easy,cheap,effective,rugged,and safe(QuEChERS)extraction and liquid chromatography-tandem mass spectrometry[J].Journal of Agricultural and Food Chemistry,2012,60(1):60-65.
[19]YAN Z,NIE J Y,XU G F,et al.Simultaneous determination of plant growth regulators in fruits using a modified QuEChERS procedure and UPLC-MS/MS[J].Horticultural Plant Journal,2016,2(4):203-208.