超高效液相色谱-串联质谱法测定豆芽中21种植物生长调节剂
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摘要
建立了超高效液相色谱-质谱/质谱法(UPLC-MS/MS)测定豆芽中多种植物生长调节剂残留量的方法。样品用酸化乙腈提取,浓缩置换试剂,经0. 2μm滤膜过滤,以C18色谱柱分离待测物,采用多反应监测(MRM)离子扫描模式,外标法进行定量,线性良好。21种植物生长调节剂的方法检出限为0. 001～0. 005 mg/kg,样品添加回收率为61. 5%～118. 3%,相对标准偏差为0. 6%～8. 3%(n=6)。该方法简单快捷,定量准确,可满足豆芽中21种植物生长调节剂的残留量检测要求。
An effective method of liquid chromatography-mass spectrometry/mass spectrometry( UPLC-MS/MS) was established to detect the residues of various plant growth regulators in bean sprouts.The samples were initially extracted with acetonitrile and concentrated,which were filtered by 0. 2 μm filter membrane afterwards. Then the eluate was separated by gradient elution with methanol-water solution of different ratio on C18( 100 mm×2. 1 mm×1. 7 μm) column.It was detected under the mode of positive multiple reactions monitoring( MRM). The external standard method was adopted for quantitative analysis,the correlation coefficients was more than 0. 990. Finally,the detection limit of 21 types of plant growth regulators,for all the samples,ranged from0. 001 to 0. 005 mg/kg,the recoveries of samples were 61. 5% to 118. 3% and the relative standard deviations were in the range of0. 6% to 8. 3%( n = 6).In conclusion,it was a simple and efficient method which can meet the requirements for residue testing of21 types of plant growth regulators in bean sprouts.
An effective method of liquid chromatography-mass spectrometry/mass spectrometry( UPLC-MS/MS) was established to detect the residues of various plant growth regulators in bean sprouts.The samples were initially extracted with acetonitrile and concentrated,which were filtered by 0. 2 μm filter membrane afterwards. Then the eluate was separated by gradient elution with methanol-water solution of different ratio on C18( 100 mm×2. 1 mm×1. 7 μm) column.It was detected under the mode of positive multiple reactions monitoring( MRM). The external standard method was adopted for quantitative analysis,the correlation coefficients was more than 0. 990. Finally,the detection limit of 21 types of plant growth regulators,for all the samples,ranged from0. 001 to 0. 005 mg/kg,the recoveries of samples were 61. 5% to 118. 3% and the relative standard deviations were in the range of0. 6% to 8. 3%( n = 6).In conclusion,it was a simple and efficient method which can meet the requirements for residue testing of21 types of plant growth regulators in bean sprouts.
引文
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[10]谢寒冰,周明莹,赵海峰,等.高效液相色谱-四级杆飞行时间质谱法同时检测豆芽中的3种外源植物激素残留[J].色谱,2014,32(5):493-498.
[2]何瑞,刘艾平,曹玉广.植物生长调节剂实用中的安全问题[J].中国卫生监督杂志,2003,10(2):99-101.
[3]孔德洋,石利利,单正军,等.萘乙酸残留的高效液相色谱法测定[J].分析测试学报,2010,29(4):382-385.
[4]PERRINE F M,ROLFE B G,HYNES M F,et al. Gas chromatography-mass spectrometry analysis of indoleacetic acid and tryptophan following aqueous chloroformate derivatisation of Rhizobium exudates[J]. Plant Physiol.Biochem.,2004,42(9):723-729.
[5]李金克,陈华君,陈少良.GC-MS内标法定量分析植物组织中的JA、IAA和ABA[J].北京林业大学学报,2010,32(5):143-148.
[6]陈红平,刘新,王川丕,等.分散固相萃取-超高压液相色谱-串联质谱法测定茶叶中赤霉素和1-萘乙酸[J].分析化学,2012,40(7):1 059-1 064.
[7]唐莉娟,谭婷,万益群.超声波提取-高效液相色谱-电喷雾离子化质谱法测定白萝卜中植物生长调节剂[J].食品科学,2012,33(14):136-141.
[8]黄何何,徐郭明,周昱,等.高效液相色谱-串联质谱法测定水果中多种天然植物生长调节剂的残留量[J].食品安全质量监测学报,2014,5(4):1 133-1 141.
[9]国家食药监总局.豆芽中植物生长调节剂:BJS 201703[S].2017-03-01.
[10]谢寒冰,周明莹,赵海峰,等.高效液相色谱-四级杆飞行时间质谱法同时检测豆芽中的3种外源植物激素残留[J].色谱,2014,32(5):493-498.