卫生研究

目的建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定豆芽中6-苄基腺嘌呤、异戊烯腺嘌呤、4-氯苯氧乙酸、4-氟苯氧乙酸、吲哚乙酸、吲哚丁酸等6种植物生长调节剂(PGR)残留量的方法。方法豆芽经乙腈及Qu ECh ERS提取包提取,C₁₈粉末净化、离心,色谱柱为WATERS ACQUITY UPLC BEH C₁₈柱(100 mm×2.1 mm,1.7μm),样液经超纯水10倍稀释后,采用三重四级杆质谱的多反应监测模式(MRM)进行测定,基质匹配标准溶液外标法定量。结果 6种PGR在各自浓度范围内线性关系良好(r>0.998)。以空白豆芽为基质进行3个水平加标回收实验,回收率为84.2%~107.5%,相对标准偏差为3.08%~12.71%(n=6),方法检出限为0.03³.0μg/kg,定量限为0.1~10.0μg/kg。结论该法操作简便、有机试剂使用量少、灵敏度高、稳定性好,适用于豆芽中6种植物生长调节剂残留量的检测要求。

Objective A method for the simultaneous determination of 6 plant growth regulator( PGR) residues in bean sprout was developed by ultra high performance liquid chromatography-tandem mass spectrometry( UPLC-MS / MS). 6-Benzylaminopurine,isopentennyladenine,4-chlorophenoxyacetic acid,4-fluorophenoxyacetic acid,indole-3-acetic acid and indole-3-butyric acid were concerned. Methods Bean sprout samples were extracted by acetonitrile and Qu ECh ERS extraction kit,purified by C₁₈ powers. After centrifugation, the sample liquids was diluted 10 times by ultrapure water. The chromatographic analysis was carried out on an waters acquity UPLC BEH C₁₈column( 100 mm × 2. 1 mm,1. 7 μm). The analyzer confirmed and quantified by mass spectrum of triple quadrupole in the multiple reaction monitoring( MRM) mode and quantified by matrix-matched external standard method. Results The calibration curves showed good linearity in each range with correlation coefficients greater than 0. 998. 3 levels spiked recoveries were carried out using blank bean sprout extraction as substrate,the recoveries ranged from 84. 2% to 107. 5%,the relative standard deviations( RSDs) ranged from3. 08% to 12. 71%. The qualitative limits of detections( S / N = 3) were 0. 03-3. 0 μg / kg and the quantitative limits( S / N = 10) were 0. 1- 10. 0 μg / kg for the 6 PGRs.Conslusion The method is simple and easy to operate,with less organic reagent,high sensitivity and good stability. It is suitable for the detection of 6 kinds of plant growth regulators in bean sprouts.