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目的采用高效液相色谱-串联质谱法建立了同时测定水果中赤霉素GA3、吲哚-3-乙酸和1-萘乙酸3种天然植物生长调剂残留的检测方法。方法样品经QuEChERS法进行预处理,以1%乙酸乙腈提取,无水硫酸镁和C18粉末净化。选用水-乙腈为流动相,C18色谱柱分离,采用Agilent AJS ESI源、负离子扫描和多反应检测模式(MRM)进行质谱检测,基质匹配标准溶液外标法定量。结果 3种天然植物生长调剂在0.005~1.000mg/L浓度范围内线性关系良好,赤霉素GA3的方法定量限(S/N=10)分别为0.010 mg/kg,吲哚-3-乙酸和1-萘乙酸均为0.005 mg/kg。对空白水果样品进行0.020、0.050、0.100 mg/kg 3个添加水平的回收实验,赤霉素GA3、吲哚-3-乙酸和1-萘乙酸的回收率分别为75.4%~109.8%、79.1%~109.3%和79.6%~112.9%,相对标准偏差(n=6)分别为3.5%~17.4%、6.5%~15.8%和4.8%~13.9%。结论该方法快速简便,定量准确,可满足水果中3种农药的残留检测要求。
OBJECTIVE To establish a method for the simultaneous determination of griseofulvin GA3, indole-3-acetic acid and 1-naphthalene acetic acid residues in fruits by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were pretreated with QuEChERS method, extracted with 1% acetic acid in acetonitrile, and purified with anhydrous magnesium sulfate and C18 powder. Separation was performed on a C18 column using water-acetonitrile as the mobile phase. The mass spectra were detected by Agilent AJS ESI source, negative ion scan and multi-reaction detection mode (MRM). The matrix matching standard solution was determined by external standard method. Results The results showed that there was a good linear relationship between the concentrations of 0.005 ~ 1.000 mg / L and the limit of quantification (GA) of GA3 (S / N = 10) of 0.010 mg / The 1-naphthalene acetic acid was 0.005 mg / kg. The recoveries of GA3, indole-3-acetic acid and 1-NAA were 75.4% -109.8% and 79.1% for the blank fruit samples at 0.020, 0.050 and 0.100 mg / kg respectively. ~ 109.3% and 79.6% ~ 112.9%, respectively. The relative standard deviations (n = 6) were 3.5% ~ 17.4%, 6.5% ~ 15.8% and 4.8% ~ 13.9%, respectively. Conclusion The method is rapid, simple and accurate. It can meet the requirements of residue detection of three kinds of pesticides in fruits.