CAJ | 학술논문

研究建立一种检测育苗基质中矮壮素和缩节胺残留的超高效液相色谱-串联质谱法（UPLC-MS/MS）分析方法。样品采用甲醇-乙酸铵水溶液直接提取,样品无需任何净化过程;在亲水作用色谱柱SeQuant ZLC-HILIC MERCK（150 mm×2.1 mm,5μm）上进行分离,再用V（乙腈）：V（含0.1%甲酸的20 m mol/L乙酸铵溶液）=6：4为流动相等梯度洗脱;电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测对定性和定量离子进行MS测定,内标法定量。结果表明：矮壮素和缩节胺的添加水平在0.2～10μg/kg的空白添加浓度范围内线性良好（r2〉0.999）,在1、2和5μg/kg添加水平范围内,平均回收率分别为105.1%～111.6%和72%～110.2%;相对标准偏差（RSD）分别为4.0%～9.2%和7.7%～12.4%,矮壮素和缩节胺2种物质检出限（LOD）为0.2μg/kg,测定低限（LOQ）为1.0μg/kg。该方法简便、快速、灵敏、准确、耐用,适合育苗基质中矮壮素和缩节胺残留的确证和定量测定。
연구건립일충검측육묘기질중왜장소화축절알잔류적초고효액상색보-천련질보법（UPLC-MS/MS）분석방법。양품채용갑순-을산안수용액직접제취,양품무수임하정화과정;재친수작용색보주SeQuant ZLC-HILIC MERCK（150 mm×2.1 mm,5μm）상진행분리,재용V（을정）：V（함0.1%갑산적20 m mol/L을산안용액）=6：4위류동상등제도세탈;전분무정리자（ESI＋）모식전리,다반응감측（MRM）모식검측대정성화정량리자진행MS측정,내표법정량。결과표명：왜장소화축절알적첨가수평재0.2～10μg/kg적공백첨가농도범위내선성량호（r2〉0.999）,재1、2화5μg/kg첨가수평범위내,평균회수솔분별위105.1%～111.6%화72%～110.2%;상대표준편차（RSD）분별위4.0%～9.2%화7.7%～12.4%,왜장소화축절알2충물질검출한（LOD）위0.2μg/kg,측정저한（LOQ）위1.0μg/kg。해방법간편、쾌속、령민、준학、내용,괄합육묘기질중왜장소화축절알잔류적학증화정량측정。
A liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） method for the quantitative determination ofchlormequat and mepiquat residues in samples from seeding cultivation products has been established.HILIC column packed with 5 μ m particles and isocratic LC conditions at acetonitrile / 0.1% formic acid in 20mmol/L ammonium acetate （6：4, V/V） were been used to detect and identify chlormequat and mepiquat residues.Samples without clean from seeding cultivation are were analyzed. The identification and quantification were achieved by using electrospray ionization in positive ion mode （ESI^＋） with multiple reaction monitoring （MRM）. The matrix-matched internal standards calibration curves were used for quantitative determination. The linear range was 0.02-10 μ g/kg, the average recoveries ranging from 72% to 111.6% with relative standard deviations in the range of 4.0%-12.4% respectively in the spiked range of 1, 2 and 5 μg/kg.The limits of detection were 0.2 μ g/kg and the limits of quantification were 1.0 μg/kg for the the two drugs.The established method is simple, rapid,sensitive and specific, and is suitable for the identification and quantification of chlormequat and mepiquat residues in seeding cultivation.