CAJ | 학술논문

目的：建立苹果中杀铃脲的超高效液相色谱-串联质谱(UPLC-MS/MS)快速测定方法。方法苹果样品通过乙腈匀浆提取,用固相萃取小柱净化,甲醇-二氯甲烷(1：19, v：v)淋洗、洗脱后,选用C18(100 mm×2.1 mm i.d.,1.7μm)作为分析柱,甲醇/1 mmol/L 乙酸铵梯度洗脱,经高效液相色谱分离,在多反应监测模式(MRM)及电喷电离方式(ESI+)下串联质谱法进行测定,基质配标准曲线定量。结果分析物在0.01~0.50 mg/L范围内有良好的线性关系,相关系数r>0.99,空白样品中分析物在添加水平为0.01、0.02、0.05 mg/kg时,平均回收率在80.0%~84.8%之间,相对标准偏差为4.9%~8.8%,定量限为0.005 mg/kg。结论本方法简单快速、灵敏度高、准确度好,能满足定量分析的要求。
목적：건립평과중살령뇨적초고효액상색보-천련질보(UPLC-MS/MS)쾌속측정방법。방법평과양품통과을정균장제취,용고상췌취소주정화,갑순-이록갑완(1：19, v：v)림세、세탈후,선용C18(100 mm×2.1 mm i.d.,1.7μm)작위분석주,갑순/1 mmol/L 을산안제도세탈,경고효액상색보분리,재다반응감측모식(MRM)급전분전리방식(ESI+)하천련질보법진행측정,기질배표준곡선정량。결과분석물재0.01~0.50 mg/L범위내유량호적선성관계,상관계수r>0.99,공백양품중분석물재첨가수평위0.01、0.02、0.05 mg/kg시,평균회수솔재80.0%~84.8%지간,상대표준편차위4.9%~8.8%,정량한위0.005 mg/kg。결론본방법간단쾌속、령민도고、준학도호,능만족정량분석적요구。
Objective An ultra performance liquid chromatography-tandem mass spectrometry analysis (UPLC-MS/MS) was established for the determination of the residues of triflumuron pesticide in apple. Me-thods The samples were extracted by ultrasonic extraction with acetonitrile and cleaned with solid-phase ex-traction. The separation was performed on a C18 column(100 mm×2.1 mm i.d., 1.7 μm), the gradient mobile phase consisting of 1 mmol /L ammonium acetate and methanol. The separation was achieved by UPLC, and then the identification and quantification were performed using MS/MS with multiple-reaction monitoring (MRM) and positive electrospray ionization (ESI+) mode. The matrix-matched external standard calibration curves were used for the quantitative analysis. Results Under the optimum conditions, the method showed a good linearity in the range of 0.005~0.50 mg/L with correlation coefficient over 0.99. The limits of quantitation (LOQ) for the pesticide residue were 0.005 mg/kg. The average recoveries of pesticides residues were 80.0%~84.8%at the spiked levels of 0.01, 0.02 mg/kg and 0.05 mg/kg with relative standard deviations (RSDs) of 4.9%~8.8%. Conclusion The method is sensitive and accuracy and it is suitable for quantitative determi-nation of triflumuron pesticides in apple.