李文博,童 颖*
(武汉药品医疗器械检验所,湖北武汉 430075)
摘要:建立分散固相萃取-高效液相色谱-串联质谱法同时测定豆芽中11种植物生长调节剂和抗生素药物残留的分析方法。样品经过1%甲酸乙腈超声提取,无水硫酸镁和C18净化,用CAPCELL C18色谱柱分离目标物,采用正负切换多反应监测(multiple reaction monitoring,MRM)离子扫描模式对其进行分析。11 种目标化合物在 2.0~100.0 μg/L范围内相关性良好(r≥0.999 3);在5、10、20 μg/kg 3个添加水平进行加样回收实验,平均回收率范围为80.7%~102.7%,相对标准偏差为1.1%~7.1%(n=6);检出限为0.04~0.25 μg/kg,定量限为0.15~0.84 μg/kg。该方法快捷简单、灵敏度好、准确度高,能够满足豆芽中11种植物生长调节剂和抗生素药物残留的检测要求。
关键词:豆芽;植物生长调节剂;抗生素类药物;分散固相萃取;高效液相色谱-串联质谱法
中图分类号:TS207.3 文献标识码:A 文章编号:1674-506X(2022)04-0123-0009
Simultaneous Determination of 11 Plant Growth Regulators and Antibiotic Residues in Bean Sprouts by DSPE-HPLC-MS/MS
LI Wenbo, TONG Ying*
(Wuhan Institute for Drug and Medical Device Control, Wuhan Hubei 430075, China)
Abstract:To develop a method for the determination of 11 plant growth regulators and antibiotic residues in bean sprouts by the dispersive solid- phase extraction-high performance liquid chromatography-tandem mass spectrometry. The samples were ultrasonically extracted with 1% formic acid in acetonitrile, and then subjected into a purification using C18 and magnesium sulfate (MgSO4). The target compounds were separated at the CAPCELL C18 column, detected by tandem mass spectrometry in positive and negative ESI modes together with multiple reaction monitoring (MRM). The calibration curves ranging from 2.0 to 100.0 μg/L showed good linearity, while the obtained correlation coefficients were larger than 0.999 3. The average recoveries were 80.7%~102.7% when using spiked levels of 5, 10 and 20 μg/kg, and the relative standard deviations ranged from 1.1% to 7.1% (n=6). Moreover,the limits of detection (LOD) and limits of quantitation (LOQ) were 0.04~0.25 μg/kg and 0.15~0.84 μg/kg, respectively. This method is simple, sensitive and accurate, and might be suitable for the determination of 11 plant growth regulators and antibiotic residues in bean sprouts.
Keywords:bean sprouts; plant growth regulator; antibiotic; dispersive solid phase extraction; high performance liquid chromatography-tandem mass spectrometry
doi:10.3969/j.issn.1674-506X.2022.04-021
收稿日期:2022-04-09
作者简介:李文博(1989-),男,硕士,主管药师。研究方向:食品质量安全研究与检验检测。
*通信作者:童颖(1989-),女,硕士,主管药师,研究方向:食品、药品质量安全控制。
引用格式:李文博,童颖.DSPE-HPLC-MS/MS法同时测定豆芽中11种植物生长调节剂和抗生素药物残留[J].食品与发酵科技,2022,58(4):123-131.
全文查看