溶剂浮选-气相色谱/质谱法测定蔬菜中氨基甲酸酯类农药残留

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.     

气相色谱-离子阱质谱法测定蔬菜中9种有机磷农药的残留量

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.     

蔬菜、水果中16种有机磷类农药多残留GC-MS分析

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。     

气相色谱/负化学电离源质谱法测定底泥中的有机氯农药

建立了气相色谱/负化学电离源质谱(GC-NCI-MS)法测定底泥中24种有机氯农药(OCPs)残留的方法.样品采用索氏提取、硅胶/氧化铝复合柱分离纯化,p,p'DDT、o,p'-DDT采用外标法定量,其余的有机氯农药均采用内标法定量.同时,对气相色谱/负化学电离源质谱(GC-NCI-MS)法与气相色谱/电子轰击离子源质...     

超声辅助固相萃取/离子阱气相色谱-质谱联用测定蔬菜中有机磷农药残留

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％.     

蔬菜农药多残留分析中基质共提物净化方法的研究

首次建立了蔬菜中常见基质干扰物的净化方法.用GC-MS分析样品提取液、确定了蔬菜农药多残留检测常见的基质干扰物.建立常见吸附剂对基质干扰物的吸附模型,以及吸附剂对农药的吸附模型.据此建立了番茄、油菜和尖椒3种蔬菜中102种农药多残留SPE净化方法和气相色谱-质谱/选择离子存储检测方法(gas chromatography-ion trap mass spectrometry/selective ion storage, GC-MS/SIS).样品用凝胶渗透色谱(GPC)去除大分子干扰物和部分色素和(或)采用石墨化碳黑(GCB) Florisil混合SPE柱去除色素和脂肪酸.在0.02 mg/kg和0.10 mg/kg两个水平,农药添加回收率为65% ～123%(除久效磷、抗蚜威和蝇毒磷),RSD不大于15%.方法检出限在2 ～30 μg/kg范围.对于其它蔬菜,只要确定样品中的基质干扰物,即可选择合适的吸附剂制备专用的SPE柱.该方法适用于含色素、脂肪酸和大分子干扰物蔬菜样品中的农药多残留分析.     

农产品中多种农药残留的气相色谱-质谱联用法测定

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。     

液下单液滴微萃取/快速气相色谱-质谱联用法测定蔬菜中多种有机磷农药残留

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。     

气相色谱-负化学源质谱法测定蔬菜中17种拟除虫菊酯类农药残留量

建立了气相色谱-负化学源质谱检测蔬菜中17种拟除虫菊酯类农药残留量的方法。样品中的目标物经乙腈提取后,用乙二胺-N-丙基甲硅烷(PSA)和石墨化炭黑填料进行分散固相萃取净化,气相色谱-负化学源质谱选择离子监测模式测定,同位素内标法定量。在甜豌豆、绿花菜和大葱基质中均未见干扰所有农药测定的现象。17种拟除虫菊酯类农药的定量限均为0.02～5 μg/kg。在10、20、30和100 μg/kg等4个添加水平下,所有农药的回收率均为71.0%～139.0%,相对标准偏差≤12.8%。该方法可作为蔬菜中17种菊酯类农残检测的确证方法。     

气相色谱-四极杆-飞行时间质谱和气相色谱-串联质谱对水果、蔬菜中208种农药残留筛查确证能力的对比

对比研究了气相色谱-串联质谱(GC-MS/MS)与气相色谱-四极杆-飞行时间质谱(GC-QTOF/MS)在水果、蔬菜中208种农药多残留检测中基质效应及方法学效能的差异,提出两种仪器在农药残留检测方面的特点和适用范围,为残留检测分析提供参考。在苹果、柑橘、番茄、黄瓜4种基质,3个添加浓度(5.0、10.0和20.0 μg/kg)下,两种仪器中均有93.0%以上的农药回收率在70%~120%范围内且相对标准偏差(RSD)≤20%(n=5)。检测灵敏度方面,绝大部分农药在两种仪器的检出限均低于5.0 μg/kg,满足各国农药残留限量的要求,且GC-MS/MS灵敏度更高,线性范围更宽,定量能力更加准确。筛查确证方面,GC-QTOF/MS在快速、高通量筛查、准确定性及非目标化合物鉴定等方面表现出了优势。     

在线凝胶渗透色谱-气相色谱/质谱法检测茶叶中的153种农药残留

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。     

Establishment of an LC-MS/MS Method for the Determination of 45 Pesticide Residues in Fruits and Vegetables from Fujian,China

Pesticide residues in food have become an important factor seriously threatening human health. Therefore, this study was conducted to determine the pesticide residues in fruits and vegetables commonly found in Fujian, China, with the aim of constructing a simple and rapid method for pesticide residue monitoring. We collected 5607 samples from local markets and analyzed them for the presence of 45 pesticide residues. A fast, easy, inexpensive, effective, robust, and safe (QuEChERS) multi-residue extraction method followed by liquid chromatography equipped with triple-quadrupole mass spectrometry (LC-MS/MS) was successfully established. This 12-min-long 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 5 to 200 mg/L, the limits of detection for all pesticides ranged from 0.02 to 1.90 μg/kg, and the limits of quantification for the pesticides were 10 μg/kg. The recovery rates for the three levels of fortification ranged from 72.0% to 118.0%, with precision values (expressed as RSD%) less than 20% for all of the investigated analytes. The results showed that 726 (12.95%) samples were contaminated with pesticide residues, 94 (1.68%) samples exceeded the maximum residue limit (MRL) of the national standard (GB 2763-2021, China), 632 (11.23%) samples were contaminated with residues below the MRL, and 4881 (87.05%) samples were pesticide residue-free. In addition, the highest number of multiple pesticide residues was observed in bananas and peppers, which were contaminated with acetamiprid, imidacloprid, pyraclostrobin, and thiacloprid.     

超高效液相色谱-串联质谱法快速检测蔬菜中248种农药残留

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（r>0.99）。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。     

Development of GC–MS/MS method for environmental monitoring of 49 pesticide residues in food commodities in Al-Rass,Al-Qassim region,Saudi Arabia

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.     

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

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。     

固相微萃取(SPME)/GC/MS测定灌溉水中的残留甲胺磷

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。     

微热助吹扫捕集-超高压液相色谱-串联质谱法快速测定蔬菜中12种半挥发性农药残留

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0.991 8～0.999 7;检出限为0.3～1.3μg/kg,定量限为1.0～4.3μg/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。     

凝胶渗透色谱净化/液相色谱-串联质谱法对动物脂肪中111种农药残留量的同时测定

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.     

Simultaneous determination of 103 pesticide residues in tea samples by LC‐MS/MS

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.     

Validation of short run time LC-ESI (+) MS/MS method for determination of twenty recommended pesticide residues in food based on QuEChERS extraction technique

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.