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浙江省食品药品检验研究院,国家药品监督管理局中成药质量评价重点实验室,国家市场监管重点实验室(功能食品质量与安全领域),浙江省市场局重点实验室(保健食品质量安全重点实验室,浙江 杭州 310052)
王峰,硕士,副主任中药师,研究方向:食品药品的质量安全控制及风险研究,E-mail:wangfeng@zjyj.org.cn
纸质出版日期:2025-02-15,
收稿日期:2024-08-18,
修回日期:2024-09-19,
录用日期:2024-11-06
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岳超,毛思浩,周霞,阮昊,刘柱,王峰.全自动QuEChERS-UPLC-MS/MS法测定麦冬中19种植物生长调节剂和杀菌剂[J].分析测试学报,2025,44(02):318-325.
YUE Chao,MAO Si-hao,ZHOU Xia,RUAN Hao,LIU Zhu,WANG Feng.Detection of 19 Plant Growth Regulators and Fungicides in Radix Ophiopogonis by Automatic QuEChERS Combined with UPLC-MS/MS[J].Journal of Instrumental Analysis,2025,44(02):318-325.
岳超,毛思浩,周霞,阮昊,刘柱,王峰.全自动QuEChERS-UPLC-MS/MS法测定麦冬中19种植物生长调节剂和杀菌剂[J].分析测试学报,2025,44(02):318-325. DOI: 10.12452/j.fxcsxb.240818322.
YUE Chao,MAO Si-hao,ZHOU Xia,RUAN Hao,LIU Zhu,WANG Feng.Detection of 19 Plant Growth Regulators and Fungicides in Radix Ophiopogonis by Automatic QuEChERS Combined with UPLC-MS/MS[J].Journal of Instrumental Analysis,2025,44(02):318-325. DOI: 10.12452/j.fxcsxb.240818322.
建立全自动QuEChERS-UPLC-MS/MS法快速测定浙麦冬中19种植物生长调节剂和杀菌剂残留量的分析方法。研究使用挥发性盐提取溶液体系联合全自动QuEChERS仪器制备样品溶液,以ACQUITY UPLC BEH C
18
色谱柱(1.7 μm,3.0 mm × 100 mm)进行分离,0.05%甲酸-2 mmol/L甲酸铵-乙腈为流动相进行梯度洗脱,采用正、负离子模式电离,保留时间依赖多反应监测(MRM)模式检测,以保留时间和离子丰度比定性,基质匹配外标法定量。结果表明,19种农药在5~200 ng/mL范围内线性关系良好,相关系数(
r
2
)均大于0.999。方法检出限为0.048~1.68 μg/kg,方法定量下限为0.16~5.61 μg/kg。19种农药在空白基质中3个加标水平浓度的回收率为62.8%~117%,相对标准偏差(RSDs,
n
=6)为1.9%~9.1%。使用该方法对30批麦冬进行检测,样品中3-吲哚乙酸、氟醚唑、烯效唑、胺鲜酯有不同程度的检出。该研究方法高效、便捷、准确,适用于麦冬中19种植物生长调节剂和杀菌剂的测定,可满足大批量检测的需求。
To establish a method for the detection of 19 plant growth regulators and fungicides in
Radix Ophiopogonis
by automatic QuEChERS method combined with ultra high pressure liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS). The sample was prepared by using the volatile salt ex
traction solution system combined with a fully automatic QuEChERS instrument. The 19 target compounds were separated on an ACQUITY UPLC BEH C
18
column(1.7 μm,3.0 mm × 100 mm) with gradient elution using 0.05% formic acid-2 mmol/L ammonium formate -acetonitrile as the mobile phase,and detected with UPLC-MS/MS instrument using the external standard method and matrix quasi curve. The results showed 19 agricultural chemicals showed good linear relationships in the ranges of 5-200 ng/mL,with correlation coefficients greater than 0.999. The limits of detection(LODs) and quantitation(LOQs) for 19 carbamate pesticides were 0.048-1.68 μg/kg and 0.16-5.61 μg/kg,respectively. A spiked recovery test was using black-matrix at three spiked levels. Good recoveries for 19 agricultural chemicals were obtained with recoveries of 62.8%-117% and RSDs(
n
=6) of 1.9%-9.1%. The method was used to detect 30 batches of Zhejiang
Radix Ophiopogonis
,some samples were found to contain 3-indoleacetic acid,tetraconazole,flucon-azole,and diethyl aminoethyl hexanoate. This method was efficient,convenient,accuracy,was suitable for the rapid detection of 19 plant growth regulators and fungicides in
Radix Ophiopogonis
,and the needs of large-scale testing.
麦冬植物生长调节剂杀菌剂全自动QuEChERS样品制备系统超高效液相色谱-串联质谱仪(UPLC-MS/MS)批量检测
Radix Ophiopogonisplant growth regulatorfungicidefully automatic QuEChERS instrumentultra high pressure liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)batch testing
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