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1.
建立了一种有效分离富集并榆测蔬菜中氨基甲酸酯类农药残留的方法,即采用溶剂浮选法(SS)对蔬菜中的氨基甲酸酯类农药残留进行分离富集.然后用气相色谱,质谱(GC/MS)进行检测.考察了浮选溶剂、试液pH、通气速度及浮选时间等因索对浮选效果的影响,得剑了优化浮选条件 对此条件下的浮选产物进行气相色谱/质谱检测,回收率为81.6%~97.8%,RSD为1.39%~2.65%,定量限(LOQ)为0.39-6.17 pg/kg.  相似文献   

2.
建立气相色谱-离子阱质谱法测定蔬菜中9种有机磷农药残留的方法.样品经乙酸乙酯提取、无水硫酸钠脱水、活性炭小柱净化,浓缩后通过气相色谱-离子阱质谱进行测定.9种有机磷农药的浓度在0.05~1.0μg/mL范围内与其对应的色谱峰面积具有良好的线性关系(r>0.999).在3个不同添加浓度下的平均回收率为76.5%~101.2%,测定结果的相对标准偏差为3.9%~9.4%(n=7).该方法快速、准确、操作简便,能满足蔬菜中有机磷农药残留的检测要求.  相似文献   

3.
蔬菜、水果中16种有机磷类农药多残留GC-MS分析   总被引:1,自引:0,他引:1  
建立了蔬菜、水果中16种农药的气相色谱-离子阱质谱多残留检测方法。采用乙腈作为提取剂,经过Florisil柱净化,用ITQ700气相色谱-离子阱质谱联用仪进行分析。以保留时间和特征离子定性、峰面积定量,确定了16种有机磷农药的线性回归方程、相关系数及最低检出限。结果表明,16种有机磷农药线性关系良好。农药添加浓度为0.5μg/mL,回收率为70%~120%,相对标准偏差20%,最低检出限在0.0012~0.02μg/g之间,符合农药多残留检测要求。此方法具有良好的回收率、精确度和准确度,干扰少,可用于实际检测。  相似文献   

4.
通过超声辅助固相萃取提取并富集蔬菜中残留的乐果和氧化乐果等9种有机磷农药,采用离子阱二级质谱定性并定量检测其含量,建立了气相色谱-质谱联用测定蔬菜中有机磷农药残留的分析方法.结果表明,所建立的方法简单,快速,灵敏度高.9种有机磷农药的检出限为0.02~0.04 μg/mL,添加回收率为75.07%~99.47%.  相似文献   

5.
果蔬中107种残留农药的气相色谱-质谱检测方法   总被引:45,自引:12,他引:33  
采用毛细管气相色谱-质谱法对果蔬中107种残留农药检测进行了系统研究,考察了被测组分在不同极性毛细管色谱柱上的保留时间值,对比了不同前处理技术对检测结果的影响,确定了气相色谱-质谱检测农残初筛离子选择原则,规定了气相色谱-质谱确证被捡出农药应符合的条件。  相似文献   

6.
综述了环境介质与生物样品中三氯生残留的检测方法研究进展。检测方法有气相色谱-质谱法、液相色谱法、液相色谱-质谱联用以及分光光度法、酶联免疫分析方法和电化学法等。气相色谱-质谱法检测三氯生线性关系良好,检出限、定量限低,精密度、准确度较高,但样品需要衍生化前处理,操作较为复杂。液相色谱法操作相对于气相色谱-质谱法更为简便,且具有选择性强、线性范围宽、定量准确和精密度高等优点,目前高效液相色谱法是大多数实验室的首选。液相色谱-质谱法是在液相色谱的基础上,采用质谱法对样品中的三氯生残留进行定性定量,定量准确,检出限低。其他方法的使用率较低,但也可满足环境介质与生物样品中三氯生残留的检测。目前乃至未来的一段时间内,环境介质及生物样品中三氯生残留的检测方法将以色谱-质谱法为主。目前仪器检测技术条件已经相对成熟,因此应积极寻找适合不同样品的前处理方法,使检测结果更加准确和精确,实验过程更加快捷方便。  相似文献   

7.
建立了液下单液滴微萃取/快速气相色谱-质谱联用测定蔬菜中多种有机磷农药残留的方法,并对前处理条件进行了优化。采用液下单液滴微萃取技术对样品进行萃取和浓缩,以快速气相色谱-质谱(GCMS)分离检测,内标法定量。在优化条件下,治螟磷、甲拌磷、异稻瘟净、甲基对硫磷、皮蝇磷、马拉硫磷、毒死蜱、水胺硫磷和喹硫磷9种有机磷农药的色谱峰分离良好,相关系数均不低于0.995 8,检出限为0.32~0.91μg/kg,加标回收率为83.2%~134.5%,相对标准偏差(n=5)为3.4%~16.5%。该方法样品前处理简单,分析快速,灵敏度高,能够应用于蔬菜中这9种有机磷农药残留的检测。  相似文献   

8.
农产品中多种农药残留的气相色谱-质谱联用法测定   总被引:4,自引:0,他引:4  
建立了同时检测大白菜、苹果、大豆和豆沙中211种农药残留的气相色谱-质谱联用法。农药经乙腈-水溶液匀质提取,C18固相萃取柱净化和PSA固相萃取柱净化,洗脱液浓缩后用丙酮-正己烷(1∶1)溶解,经HP-5MS石英毛细管柱分离后,用气相色谱-质谱联用仪采用选择离子扫描方式测定,外标法定量。结果表明211种农药在0.05~0.5 mg/L范围内线性关系良好,相关系数为0.975~0.998,其定量下限为0.002~0.020 mg/kg。在0.1 mg/kg加标水平下,211种农药在大白菜、苹果、大豆和豆沙中的平均回收率为67%~117%,相对标准偏差为1.1%~23.8%。该方法操作简单、净化效果好、灵敏度高,适用于蔬菜、水果等农产品中多种农药残留的测定。  相似文献   

9.
蔬菜中有机磷和氨基甲酸酯类农药多残留联合检测方法   总被引:2,自引:0,他引:2  
有机磷和氨基甲酸酯类农药是蔬菜生产中常用的杀虫剂,我国70%的有机磷杀虫剂是剧毒、高毒农药。农药如果使用不当,不但药效不好,还会发生药害,污染环境,造成人畜中毒。因此,加强对农药残留的监控,禁止农药残留超标的蔬菜进入市场,确保消费安全已成为当务之急。本文报道用毛细管气相色谱法测定蔬菜中有机磷和氨基甲酸酯类农药多残留的联合检测方法。  相似文献   

10.
高分辨质谱技术在农药残留检测中的应用   总被引:3,自引:0,他引:3  
农药残留检测是农产品中有害物质控制的重要组成部分,随着农药残留限量标准体系的发展完善,农药残留检测方法也在不断进步。近年来质谱技术发展迅速,已被广泛应用于农药残留检测领域,高分辨质谱由于具有较高的分辨率和质量精确度,在复杂基质的农药多残留高通量检测中发挥着越来越重要的作用。本文从高分辨质谱与液相色谱、气相色谱及其他分离模式联用等方面出发,简述了近5年来高分辨质谱在农药残留检测中的应用,对目前高分辨质谱在农药残留检测应用中发现的问题进行了讨论,并对其未来发展趋势进行展望。  相似文献   

11.
李军明  钟读波  王亚琴  冯雷  祝红昆 《色谱》2010,28(9):840-848
建立了在线凝胶渗透色谱-气相色谱/质谱(GPC-GC/MS)分析茶叶中153种农药残留的方法。样品用乙腈超声提取,提取液经石墨化炭黑固相萃取柱净化后,经GPC-GC/MS在线净化、分离和检测。方法的加标回收率为73.32%~117.05%,相对标准偏差为0.76%~13.18%。方法的检出限和定量限范围分别为0.0003~0.006 mg/kg和0.001~0.02 mg/kg。该方法样品前处理简单、分析时间短,灵敏度和精密度均符合农药多残留检测技术的要求,适用于茶叶中多种农药残留的检测。  相似文献   

12.
The harmful effects of pesticide residues are a threat to our health. Therefore, the current study aimed to validate a simple method for the determination of pesticide residues in commonly consumed fruits and vegetables from Al-Rass, Al-Qassim region, Saudi Arabia. A total of 1430 samples were collected from a local market and then analyzed for monitoring of 49 pesticide residues. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) multi-residue extraction method followed by gas chromatography equipped with triple-quadrupole mass spectrometry (GC–MS/MS) was successfully implemented. This 17-min-run analytical method detects and quantifies pesticide residues with acceptable validation performance parameters in terms of sensitivity, selectivity, linearity, the limit of quantification, accuracy, and precision. The linear range of the calibration curves ranged from 10 to 300 µg/L, all the pesticide LODs ranged from 0.0005 to 0.0024 mg/kg, and the pesticide LOQs ranged from 0.0011 to 0.0047 mg/kg. The recovery values at the three fortification levels ranged from 78 % to 107 %, and the precision values (expressed as RSD%) were less than 20 % for all of the investigated analytes. The results showed that 138 (9.65 %) of the analyzed samples were contaminated with pesticide residues, 40 (2.80 %) of the analyzed samples exceeded the maximum residue limit (MRL) of the European Commission regulations (EC) for pesticides residues, 98 (6.85 %) of the analyzed samples were contaminated with residues below the MRL, and 1292 (90.35 %) of the analyzed samples were pesticide residue-free. Coriander contained the highest percentage (46.88 %) of pesticide residues, particularly tetradifon that representing 18.75 % noncompliance with the MRL, followed by parsley, with 20.59 % pesticide residues (10.29 % non-compliance). Multiple pesticide residues were observed most frequently in tomatoes and dates which were contaminated with buprofezin and ethion respectively.  相似文献   

13.
采用超高效液相色谱-串联质谱(UHPLC-MS/MS)技术建立了快速检测蔬菜中248种农药残留的分析方法。蔬菜样品采用乙腈提取,盐析后无需净化,缩短了样品前处理的时间。采用正负离子多反应监测(MRM)模式对蔬菜中248种农药残留进行定性和定量分析。245种农药在各自的线性范围内线性关系良好(r0.99)。除丁硫克百威、灭蝇胺、苯磺隆和二氯喹啉酸4种农药外,其余244种农药在3个添加水平下的平均回收率范围为63.0%~126.4%,相对标准偏差(RSD)范围为0.5%~26.7%,方法的定量限为0.001~0.030 mg/kg。该方法具有简单、快速、灵敏度高、准确度高等优点,适合蔬菜样品中农药多残留的快速检测分析。  相似文献   

14.
采用超高效液相色谱–串联质谱法测定生活饮用水中10种农药残留。水样直接进样,选用Waters ACQUITY UPLC~BEH C_(18)柱分离,以乙腈–0.1%甲酸溶液为流动相进行梯度洗脱,质谱选用多反应监测模式分析,10种农药的质量浓度在0.5~50μg/L范围内与色谱峰面积呈线性相关,检出限(3S/N)在0.03~0.50μg/L之间,测定值的相对标准偏差在1.14%~9.91%之间,加标回收率在91.6%~107.1%之间。该法简便准确,适用于生活饮用水中农药残留的检测。  相似文献   

15.
陈正毅  李运达  张卓旻  李攻科 《色谱》2020,38(1):120-126
将微热助吹扫捕集技术与超高压液相色谱-串联质谱(UHPLC-MS/MS)结合,建立了蔬菜中12种半挥发性农药残留的快速分析方法。系统优化了前处理条件,在10 min内即可完成样品前处理过程。12种半挥发性农药残留在各自范围内线性关系良好,相关系数(R2)为0.9918~0.9997;检出限为0.3~1.3 μg/kg,定量限为1.0~4.3 μg/kg。实际样品的加标回收率为80.0%~120.0%,日内和日间精密度均小于10%。该方法具有基质净化效果好、前处理过程简单和分析速度快等优点,可用于蔬菜中多种半挥发农药残留的同时快速分析。  相似文献   

16.
固相微萃取(SPME)/GC/MS测定灌溉水中的残留甲胺磷   总被引:7,自引:0,他引:7  
农药残留是当前农产品出口及内销中的最大卫生质量问题,由水携带是农药残留的来源之一。本文利用SPME/GC/MS技术对灌溉用水农药残留进行了分析研究,对固相微萃取条件进行了选择,并作了加入回收实验,测定了水中的甲胺磷含量。  相似文献   

17.
A simple and sensitive method was developed and validated for the simultaneous determination of 103 pesticide residues in tea by LC‐MS/MS. For the analysis of the pesticide with polarity, thermal lability or low volatility, this LC‐MS/MS method has an advantage over GC. In this work, residual pesticides were extracted from the tea sample with ACN and then purified using Carb‐NH2 SPE cartridges. Using the multiple reaction monitoring mode, the pesticides were quantified and identified by the most abundant and characteristic fragment ions. The recoveries obtained for each pesticide ranged between 65 and 114% at three spiked concentration levels. The intra‐day precisions were lower than 19.6%. Good linear relationships were observed with the correlation coefficients r2 >0.996 for all analytes. The established method was successfully applied to the determination of pesticide residues in real tea samples.  相似文献   

18.
建立了液相色谱-串联质谱法同时测定动物脂肪中111种农药残留的分析方法.样品经乙腈均质提取2次,旋转蒸发浓缩后经过凝胶渗透色谱净化.111种农药在Atlantis T3柱上以乙腈和0.1%甲酸溶液为流动相,梯度洗脱条件下完成分离,采用电喷雾电离串联质谱在正离子多反应监测模式下进行测定.目标化合物的保留时间为2.4 ~33.8 min,线性相关系数为0.984 5 ~0.999 9;在4种动物脂肪中分别添加1倍、2倍、4倍定量下限3个水平的平均回收率为60% ~120%,相对标准偏差为0.6% ~19.8%;111种农药在动物脂肪中的检出限为0.20 ~960 μg/kg,定量下限为0.40 ~2 400 μg/kg.该方法操作简单、灵敏度高、选择性好,符合农药多残留分析的要求.  相似文献   

19.
Food is expected to contain pesticide residues that might have many problems due to their toxicities for human and animals. So, it is very important to detect and quantify the pesticides contamination levels to increase food safety for the human. The target of our study is to analyse a 20 new pesticides including different pesticide classes such as 1 acaricide, 3 fungicides, 2 plant growth regulators, 11 herbicides, 1 insecticide, 1 rodenticide, and 1 metabolite which were selected according to their modern application in the Egyptian agriculture as well as the recommendation of the Egyptian Agriculture Pesticides Committee (APC). The research is focused on the method validation for the routine analysis of the targeted pesticide residues according to the European SANTE/11,813/2017 guideline. The validation was carried out by fortifying of three levels at 0.01, 0.05 and 0.1 mg/kg in four blank matrices: apple, green beans, fennel seeds and rice which represent different classes of food. The most common citrate buffered QuEChERS extraction method and liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS/MS) device were used. The mass spectrometer was operated in the positive electrospray ionisation ESI (+) mode and the non-scheduled multiple reactions monitoring (MRM) method in a short run time of 16.0 min. The limits of quantifications (LOQs) for all pesticides ranged between 0.01 and 0.05 mg/kg. Good linearity of the method was in the concentration range 0.001–0.5 μg/ml with acceptable correlation coefficients (r2) ≥ 0.99 for all analytes. The average recoveries for all the target pesticide residues were in the range of 70–120% with relative standard deviations RSDs ≤ 20%. The matrix effect was compensated by using the standard addition method. This short run time LC ESI (+) MS/MS Method may help laboratories which deal with the routine pesticide residues analysis in different food samples.  相似文献   

20.
A multiresidue method based on extraction with ethyl acetate has been used at the Swedish National Food Administration since 1989 to monitor pesticide residues in fruit and vegetables. The method has been continuously adjusted, resulting in simple and quick analyses of pesticide residues. To recover basic pesticides, the addition of an alkali is necessary. The addition of sodium hydrogen carbonate has been shown to recover all pesticides effectively without any degradation. The liquid chromatography (LC) with tandem mass spectrometry (MS/MS) technique has made it possible to analyse more polar pesticides and to replace many single methods. The latest development in the multiresidue method, comprising the use of gas chromatography (GC) with MS/MS, has further improved the analysis by replacing the conventional GC detectors. The need for cleanup has been reduced or eliminated entirely. Consequently, the method has been simplified in a way that makes it possible to recover all included analytes in many different matrices in one single extraction and to detect them either with GC-MS/MS or with LC-MS/MS.  相似文献   

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