CAJ | 학술논문

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0.005～1.000 mg/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。
목적：채용고효액상색보-천련질보법건립료동시측정수과중적매소GA3、신타-3-을산화1-내을산3충천연식물생장조제잔류적검측방법。방법양품경QuEChERS법진행예처리,이1%을산을정제취,무수류산미화C18분말정화。선용수-을정위류동상, C18색보주분리,채용Agilent AJS ESI원、부리자소묘화다반응검측모식(MRM)진행질보검측,기질필배표준용액외표법정량。결과3충천연식물생장조제재0.005～1.000 mg/L농도범위내선성관계량호,적매소GA3적방법정량한(S/N=10)분별위0.010 mg/kg,신타-3-을산화1-내을산균위0.005 mg/kg。대공백수과양품진행0.020、0.050、0.100 mg/kg 3개첨가수평적회수실험,적매소GA3、신타-3-을산화1-내을산적회수솔분별위75.4%～109.8%、79.1%～109.3%화79.6%～112.9%,상대표준편차(n=6)분별위3.5%～17.4%、6.5%～15.8%화4.8%～13.9%。결론해방법쾌속간편,정량준학,가만족수과중3충농약적잔류검측요구。
Objective To develop a method for the simultaneous detection of GA3, IAA and NAA in fruits by QuEChERS-HPLC-ESI-MS/MS. Methods The samples were extracted with acetonitrile with 1%acetic acid, purified using powder of magnesium sulfate and C18. Three pesticides were separated on a C18 column with the mobile phases of water and acetonitrile and finally detected with negative electrospray io-nization in MRM mode. The matrix-matched external standard calibration curves were used for quantitative analysis. Results The linearities of GA3, IAA and NAA were in the concentration ranges of 0.005～1.000 mg/L, with the correlation coefficients higher than 0.9990 for the 3 pesticides. The limit of quantification (LOQ) were 0.010 mg/kg for GA3, 0.005 mg/kg for IAA and NAA. For all the samples, the mean spiked re-coveries of GA3, IAA and NAA ranged from 75.4%～109.8%, 79.1%～109.3% and 79.6%～112.9%, respec-tively, and the relative standard deviations (RSD, n=6) were in the range of 3.5%～17.4%, 6.5%～15.8% and 4.8%～13.9%, respectively. Conclusion The method is quick, easy, effective, sensitive and accurate, and it can meet the requirements for the determination of GA3, IAA and NAA pesticide residues in fruits.