摘要
目的建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定柑橘中多菌灵、噻菌灵、嘧霉胺、抑霉唑、甲基硫菌灵、咪鲜胺、对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯、对羟基苯甲酸丁酯和2,4-D的分析方法。方法用乙腈作为提取剂,振摇30 min后加入5 g氯化钠静置30 min,上清液过滤待UPLC-MS/MS分析。采用ACQUITY UPLC BEH C18柱(2.1 mm×100 mm,1.7μm)进行液相色谱分离,以0.1%甲酸0.5 mmol/L甲酸铵和甲醇作为流动相进行梯度洗脱。采用多反应监测模式进行质谱测定,以基质配制标准溶液外标法定量。结果11种保鲜剂在1.0~100μg/L范围内线性关系良好(r^2>0.999),方法最低检出限为0.03~0.21μg/kg,最低定量限为0.07~0.5μg/kg;在3个添加水平为1.0、5.0、10.0μg/kg时,回收率为75.1%~110.4%,相对偏差为0.4%~9.8%。对26个柑橘样品进行分析,多菌灵、咪鲜胺和对羟基苯甲酸丙酯在所有样品中均有检出,2,4-D在25个样品中有检出,嘧霉胺检出率最低,仅在一个样品中检出。从品种上看,柠檬的平均用药量最大(2285.51μg/kg),其次是橙类、橘类、柑类和金橘。结论该方法简便、灵敏、准确,适用于柑橘中多种保鲜剂的同时测定。
Objective To establish a method of determination of carbendazim,thiabendazole,pyrimethanil,imazalil,thiophanate,prochloraz,methylparaben,ethyl p-hydroxybenzoate,propyl p-hydroxybenzoate,butyl p-hydroxybenzoate and 2,4-D. in citrus by ultra performance liquid chromatography-tandem mass spectrometry(UTS-MS/MS). Methods The sample was treated with acetonitrile as extractant. After shaking for 30 min,5 g of sodium chloride was added and allowed to stand for 30 min. The liquid chromatographic separation was carried out using an ACQUITY UPLC BEH C18 column(2.1 mm × 100 mm,1.7 μm) with gradient elution with 0.1% formic acid 0.5 mmol/L ammonium formate and methanol as mobile phase. Mass spectrometry was performed using a multi-reaction monitoring mode and quantified by matrix preparation of standard solution external standards. Results The linearity of 11 kinds of preservatives in the range of 1.0-100 μg/L was good(r^2>0.999). The minimum detection limit of the method was 0.03-0.21 μg/kg,and the lowest limit of quantification was 0.07-0.5 μg/kg. At 1.0,5.0,and 10.0 μg/kg,the recoveries were75.1% to 110.4%,and the relative standard deviations were 0.4% to 9.8%. Analysis of 26 citrus samples,carbendazim,prochloraz and propylparaben were detected in all samples,2,4-D was detected in 25 samples,and pyrimethanil was detected in one sample. In terms of variety,the average dosage of lemon was the highest(2285.51 μg/kg),followed by orange,orange,citrus and kumquat. Conclusion This method is simple,sensitive and accurate,which is suitable for simultaneous determination of various preservatives in citrus.
作者
李曦
唐春燕
仲伶俐
雷欣宇
赵珊
魏超
LI Xi;TANG Chun-Yan;ZHONG Ling-Li;LEI Xin-Yu;ZHAO Shan;WEI Chao(Analysis and Determination Center,Sichuan Academy of Agricultural Sciences,Chengdu 610066,China)
出处
《食品安全质量检测学报》
CAS
2019年第24期8382-8388,共7页
Journal of Food Safety and Quality
关键词
超高效液相色谱-串联质谱法
保鲜剂
柑橘
ultra performance liquid chromatography-tandem mass spectrometry
preservatives
citrus
