共查询到20条相似文献,搜索用时 15 毫秒
1.
Martínez Vidal JL Fernández Moreno JL Arrebola Liébanas FJ Garrido Frenich A 《Journal of AOAC International》2007,90(4):1146-1164
A multiresidue method has been developed for determining pesticide residues in the tropical fruits kiwi, custard apple, and mango. The intended purpose of the method is for regulatory analyses of commodities for pesticides that have established maximum residue limits. A fast and simple extraction method with cyclohexane-ethyl acetate (1 + 1, v/v) and a high-speed homogenizer was optimized. Pressurized liquid extraction was evaluated as an alternative automated extraction technique. The pesticide residues were determined by using low-pressure gas chromatography coupled to tandem mass spectrometry. The proposed methodology was validated for each matrix. Pesticide recoveries ranged from 70 to 110%, with repeatability relative standard deviations of < or = 18% at spiking levels of 12 and 50 microg/kg. The limits of quantitation were in the range of 0.03-6.17 microg/kg, and the limits of detection were between 0.01 and 3.75 microg/kg. Mango can be selected as a representative matrix for calibration on the basis of the results of a potential matrix effect study. The method was successfully applied to the determination of pesticide residues in real samples in Spain. 相似文献
2.
We developed and evaluated a new method of low-pressure gas chromatography-tandem mass spectrometry (LP-GC/MS-MS) using a triple quadrupole instrument for fast analysis of 150 relevant pesticides in four representative fruits and vegetables. This LP-GC (vacuum outlet) approach entails coupling a 10 m, 0.53 mm i.d., 1 μm film analytical column between the MS transfer line and a 3 m, 0.15 mm i.d. capillary at the inlet. The MS creates a vacuum in the 10 m analytical column, which reduces the viscosity of the He carrier gas and thereby shifts the optimal flow rate to greater velocity. By taking advantage of the H(2)-like properties of He under vacuum, the short analytical column, a rapid oven temperature ramp rate, and the high selectivity and sensitivity of MS/MS, 150 pesticides were separated in <6.5 min. The 2.5 ms dwell time and 1 ms interscan delay of the MS/MS instrument were critical for achieving >8 data points across the 2-3 s wide peaks. To keep dwell and cycle times constant across all peaks, each segment consisted of 30 analytes (60 transitions). For assessment, we injected extracts of spiked broccoli, cantaloupe, lemon, and sweet potato from the updated QuEChERS sample preparation method. Average recoveries (n=72) were 70-120% for 144 of the pesticides, and reproducibilities were <20% RSD for all but 4 analytes. Also, detection limits were <5 ng/g for all but a few pesticides, depending on the matrix. In addition to high quality performance, the method gave excellent reliability and high sample throughput, including easy peak integration to obtain rapid results. 相似文献
3.
In this study, the feasibility of low-pressure gas chromatography (LP-GC) in conjunction with a triple quadrupole mass spectrometer, as a route towards fast pesticide residue analysis, was investigated. A Varian GC-MS system equipped with a mass spectrometer model 1200 was used. LP-GC-MS experiments were performed on a HP-5 10 m x 0.32 mm x 0.25 microm analytical column connected to a 2.5 m x 0.15 mm non-coated restriction precolumn at the inlet end. For comparison purposes conventional GC-MS analysis was performed on a RTX-5 30 m x 0.25 mm x 0.5 microm column. Under the optimized conditions the analysis time was reduced to 13.3 min with the LP-GC approach which corresponds to an almost threefold gain in speed versus the conventional GC (37 min). Despite the poorer separation power of the LP-GC column, the experiments conducted with tomato and onion extracts spiked with 78 pesticides proved that LP-GC-MS is of practical value to perform full scan screening analysis. Moreover, the rate of false negative results was higher in the case of conventional GC-MS while the LP-GC-MS enabled correct identification of pesticides at lower levels since the peaks were improved in both size and shape. Validation experiments were performed on a sample of 12 representative pesticides for comparison of performance characteristics of the LP-GC and GC approaches with mass spectrometer operated in scan, SIM and MS/MS mode. The LP-GC column set-up interfaced to the MS detector was found to be superior to the conventional GC with respect to obtained linearity, accuracy and precision parameters. Also, lower limits of detection in real extracts were achieved using the LP-GC approach. Finally, the LP-GC-MS/MS analysis of tomato samples with incurred pesticide residues demonstrated the applicability of the developed method for analysis of real samples. 相似文献
4.
Martínez Vidal JL Arrebola FJ Mateu-Sánchez M 《Rapid communications in mass spectrometry : RCM》2002,16(11):1106-1115
The use of gas chromatography/tandem mass spectrometry (GC/MS/MS) applied to determine multiple pesticide residues in fresh vegetables has been thoroughly studied. A single injection method to detect, confirm and quantify 54 multiclass pesticides has been developed and applied in a routine analysis laboratory. The proposed method consists of a rapid extraction of 15 g of vegetable sample with dichloromethane. An additional clean-up step is not necessary even when injecting 10 microL of extract. Instead the gas chromatograph was fitted with a carbofrit inserted into the glass liner and a guard column. In addition, the detection mode chosen (MS/MS) provides additional selectivity. The method has been validated and applied to 1300 samples in a routine laboratory following specified quality criteria. The recovery efficiencies obtained for all the pesticides ranged between 70.2 and 110.8% at two different fortification levels. The relative standard deviation for quantification (RSD) was lower than 16.7% for all the compounds. Important experimental parameters, such as the conditioning of carbofrit, overload of the analytical column, and cleanliness of the ion trap, were evaluated for their influence on the performance of the method. 相似文献
5.
González-Rodríguez MJ Garrido-Frenich A Arrebola FJ Martínez-Vidal JL 《Rapid communications in mass spectrometry : RCM》2002,16(12):1216-1224
A rapid multiresidue method for the analysis of 72 pesticides has been developed using a single injection with low-pressure gas chromatography/tandem mass spectrometry (LP-GC/MS/MS). The LP-GC/MS/MS method used a short capillary column of 10 m x 0.53 mm i.d. x 0.25 microm film thickness coupled with a 0.6 m x 0.10 mm i.d. restriction at the inlet end. Optimal LP-GC conditions were determined which achieved the fastest separation in MS/MS detection mode. Also MS/MS conditions were optimized in order to increase sensitivity and selectivity. The analytical parameters of the LP-GC/MS/MS method were compared with those obtained by GC/MS/MS using a conventional capillary column (30 m x 0.25 mm i.d. x 0.25 microm film thickness). Better precision and sensitivity values were obtained with the LP-GC/MS/MS approach. The limits of detection (LOD) of the compounds ranged from 0.1 to 14.1 microg L(-1) for LP-GC/MS/MS, lower than those obtained for conventional GC/MS/MS that ranged from 0.1 to 17.5 microg L(-1). The peak widths obtained with the short column in LP-GC are similar to those obtained using conventional capillary GC columns, and the peaks can be successfully identified by MS/MS detection with the conventional scan speed of ion-trap instruments. In addition, the analysis time was significantly reduced with LP-GC/MS/MS (32 min) versus GC/MS/MS (72 min), allowing the number of samples analyzed per day in a routine laboratory to be doubled. 相似文献
6.
分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药的残留量 总被引:11,自引:0,他引:11
采用分散固相萃取-气相色谱-串联质谱(QuEChERS-GC-MS/MS)建立了蔬菜中107种农药残留量的分析方法。样品由含1%冰醋酸的正己烷饱和乙腈提取、分散固相萃取法净化,采用气相色谱-串联质谱方法在分时段选择反应监测模式下进行测定,外标法定量。所有农药在0.05~1 mg/L范围内线性关系均良好;所有农药的方法定量限(LOQ)均低于10 μg/kg;在10 μg/kg的添加水平下,大蒜、青刀豆、萝卜和菠菜4种基质中绝大多数农药的平均回收率处于60%~130%之间,相对标准偏差(RSD)不大于15.3%。该方法不仅能用于多种蔬菜基质中107种农药残留的检测,而且还能较好地解决本底成分相当复杂的大蒜基质极易出现的干扰问题。 相似文献
7.
Martínez Vidal JL González-Rodríguez MJ Arrebola FJ Frenich AG Sánchez López FJ Mora Díez N 《Journal of AOAC International》2003,86(4):856-867
A selective and reliable extraction procedure was developed and validated to determine multiclass pesticide residues in lyophilized agricultural plants by low-pressure gas chromatography coupled with tandem mass spectrometry. The method is based on a rapid and simple extraction of the lyophilized sample with dichloromethane. The results were compared with those obtained by using fresh and naturally dried samples. Slightly better recoveries and precision values were obtained for the lyophilized samples. The application of the proposed methodology was tested by analyzing French bean plants from an agricultural area of Almería (Spain). The availability of this methodology, which is capable of detecting a high number of analytes in a single analysis, has priority in analyses for a large number of pesticides used on individual commodities. 相似文献
8.
Application of gas chromatography-tandem mass spectrometry to the analysis of pesticides in fruits and vegetables 总被引:3,自引:0,他引:3
A new analytical method was devised using gas chromatography with tandem mass spectrometry (GC-MS-MS) for the routine analysis of 31 multi-class pesticide residues and approximately 8000 fresh fruit and vegetable samples (green bean, cucumber, pepper, tomato, eggplant, watermelon, melon, and marrow). Extraction of the pesticides with dichloromethane was carried out. The optimal ionization mode, either electron impact or chemical ionization, was selected for each pesticide in the same run. Carbofrit was used in the liner and combined with the selectivity of the detector this avoided additional clean-up. Thus, not only was money and time saved, the uncertainty of the method was decreased in its application to routine analysis. The average recoveries in cucumber obtained for each pesticide ranged between 71 and 119% at two different fortification levels (n=10 each) that ranged between 7 and 300 ng g(-1) (depending on the pesticide). The relative standard deviation was lower than 19% for all compounds tested. The calculated limits of detection and quantification were typically <1 ng g(-1) which were much lower than the maximum residue levels established by European legislations. 相似文献
9.
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 总被引:5,自引:0,他引:5
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。 相似文献
10.
采用气相色谱-串联质谱(GC-MS/MS)分析技术,建立了高灵敏度检测茶叶中88种农药残留量的方法。目标化合物经加速溶剂萃取(ASE), Carb/NH2净化小柱净化,乙腈-甲苯(3:1, v/v)洗脱,采用GC-MS/MS测定。对方法的准确性、精密度、线性范围、最低检出限(LOD)和定量限(LOQ)进行了测试。其中87.5%的农药在低水平(6.4 μg/kg)的加标回收率为70%~100%; 87.5%的农药的相对标准偏差(RSD)小于15%。每个化合物均采用灵敏度最高的离子对进行定量,并采用空白茶叶基质配制标准工作液。LOQ以10倍信噪比(S/N=10)计算,86.4%农药的LOQ值低于10 μg/kg。该方法灵敏度高、准确、可靠,适用于绿茶、乌龙茶、红茶以及普洱茶中多种农药残留量的检测。 相似文献
11.
超高效液相色谱-串联质谱法快速测定蔬菜中7种氨基甲酸酯类农药残留 总被引:2,自引:0,他引:2
采用超高效液相色谱-串联质谱联用(UPLC-MS/MS)技术建立了同时检测蔬菜中7种氨基甲酸酯类农药多残留量的快速检测方法。样品经乙腈提取,氨基固相萃取柱净化,WatersC18超高效液相色谱柱分离,进入电喷雾串联四极杆质谱进行检测,采用多反应监测(MRM)分析,对液质分离条件和样品前处理条件进行了优化。结果表明7种氨基甲酸酯类农药在2~500μg/L范围内线性良好(r≥0.9986)。在0.005~0.01mg/kg范围内,平均加标回收率在72.4%~112.1%之间;相对标准偏差小于13%。该方法检出限范围为1.31~3.72μg/L,测定结果满足多残留农残的检测要求。 相似文献
12.
气相色谱-串联质谱技术分析烟草中的132种农药残留 总被引:3,自引:0,他引:3
利用气相色谱-串联质谱(GC-MS/MS)检测技术,建立了检测烟草中的132种农药残留的高灵敏度方法。分析过程中考察了不同萃取溶剂、不同缓冲盐体系、不同净化剂对目标物回收率的影响。最终确定烟草样品以乙腈进行提取,以N-丙基乙二胺(PSA)与碳18(C18E)的混合净化剂进行净化,氮气吹近干后用正己烷-丙酮(9:1, v/v)复溶,过有机滤膜后进行GC-MS/MS测定,内标法定量。132种农药在20~2000 μg/kg之间线性关系良好(r2 >0.99);所有农药的方法定量限(LOQ, S/N=10)均低于20 μg/kg;在50、200、500 μg/kg的加标水平下,除灭蚁灵及六氯苯回收率稍低外,其他农药的平均回收率为68.10%~123.15%,相对标准偏差(RSD)为1.79%~19.88%。对国际烟草科学研究合作中心(CORESTA)2012年共同实验的烟草样品进行检测,对比本方法与已有的标准方法,其结果一致性较好。该方法准确、可靠,灵敏度好,适用于烟草中132种农药残留的快速筛查与定性、定量分析。 相似文献
13.
QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中41种农药残留 总被引:7,自引:0,他引:7
采用QuEChERS-超高效液相色谱-串联质谱技术,建立了蔬菜中常见的隐性农药、禁限用农药、植物生长调节剂等检出率较高的41种农药残留的测定方法。蔬菜样品用1%(v/v)乙酸-乙腈溶液提取,乙二胺-N-丙基硅烷(PSA)净化后直接进样分析,采用正、负离子多反应监测(MRM)模式,外标法定量。结果表明,在优化后的QuEChERS、色谱和质谱条件下,41种农药在1.0~100 μg/L范围内线性关系良好,相关系数(r2)大于0.999,检出限为0.003~1.00 μg/kg,不同基质中的平均回收率范围为74.1%~120.4%,相对标准偏差(RSD)范围为2.8%~11.9%。该方法快速简便、灵敏度高、净化效果好,可用于蔬菜中41种农药的快速测定,为蔬菜质量安全风险评估工作提供了有力保障。 相似文献
14.
气相色谱-串联质谱技术分析烟草中49种农药残留 总被引:1,自引:0,他引:1
采用改进的QuEChERS(quick, easy, cheap, effective, rugged and safe)前处理法,结合气相色谱-串联质谱(GC-MS/MS)技术建立了检测烟草中49种农药残留的分析方法。样品用含0.1%乙酸的乙腈溶液提取,提取液被氮吹至干后,残渣用乙腈-乙酸乙酯(1:1, v/v)溶液溶解,溶解液经N-丙基乙二胺(PSA)吸附剂、无水MgSO4、C18吸附剂净化后,直接进行GC-MS/MS测定,内标法定量。实验结果表明,49种农药在低质量浓度(0.05 μg/L)的加标水平下的平均加标回收率为60.4%~104.8%,高质量浓度(5 μg/L)的平均加标回收率为70%~115%,相对标准偏差均小于15%;其中16种农药的方法检出限(LOD)分别为0.01~0.03 μg/kg,其余33种农药的LOD均小于0.01 μg/kg;相关系数都大于或等于0.991。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痕量检测技术的要求,适用于烟草中多种农药残留的检测。 相似文献
15.
QuEChERS-液相色谱-串联质谱法同时测定果蔬中16种农药残留 总被引:5,自引:0,他引:5
建立了果蔬中吡虫啉、咪鲜胺、苯醚甲环唑、嘧菌酯、噻虫嗪等16种常见农药多残留的液相色谱-串联质谱(LC-MS/MS)分析方法。以乙腈为提取剂,样品经高速匀浆方法提取后,提取液采用液-液萃取静置分层,取上清液进行净化处理。比较了石墨化碳-氨基复合固相萃取与QuEChERS两种不同净化技术的净化效果,最终确定采用QuEChERS方法为净化手段。即提取液经装有150 mg N-丙基乙二胺(PSA)填料、900 mg无水硫酸镁的净化管净化,除去样品中大部分的色素及有机酸等干扰基质,再经LC-MS/MS分析,有效地降低了样品中的复杂基质所带来的背景干扰。加标水平为5、10、20 μg/kg时,16种农药的平均回收率为75%~111%,相对标准偏差小于16%。16种农药的检出限为0.2~5 μg/kg。采用LC-MS/MS定性分析、基质匹配标准曲线法定量分析,线性关系和回收率结果均令人满意。实验证明,建立的QuEChERS净化与LC-MS/MS相结合的检测方法具有快速、准确、灵敏度高等优点,能够准确测定果蔬中16种农药残留。 相似文献
16.
QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留 总被引:1,自引:0,他引:1
以QuEChERS为前处理方法,超高效液相色谱-串联质谱为检测仪器,建立了蔬菜中250种农药残留的快速筛查检测方法。采用含1%(v/v)乙酸的乙腈溶液提取样品,以无水硫酸镁(MgSO4)作为脱水剂,经MgSO4、丙基乙二胺(PSA)、石墨化碳(GCB)、C18混合净化剂净化,Waters ACQUITYTM UPLC BEH C18柱(100 mm×2.1 mm, 1.7 μ m)分离,超高效液相色谱-串联质谱进行测定。实验详细考察了MgSO4、PSA、GCB、C18用量对农药添加回收率的影响,结果表明,2 mL提取上清液中加入300 mg MgSO4、200 mg PSA、10 mg GCB和100 mg C18时净化效果最好。250种农药在韭菜中3个添加水平下的回收率为60.1%~120.0%,相对标准偏差(RSD)为3.5%~19.5%;检出限为0.01~50.00 μ g/kg。该方法简便、快速、可靠,可用于蔬菜中多种农药残留的快速筛查与确证的日常工作中,具有一定的推广价值。 相似文献
17.
18.
气相色谱-三重四极杆串联质谱法快速测定蔬菜水果中129种农药的残留量 总被引:5,自引:0,他引:5
采用QuEChERS方法结合气相色谱-串联质谱法(GC-MS/MS)建立了蔬菜、水果中129种农药残留同时检测的分析方法。试样用1%乙酸乙腈均质提取,采用混合型固相分散萃取剂净化后,用GC-MS/MS在多反应离子监测(MRM)模式下进行检测,外标法定量。结果表明,129种药物在一定的含量范围内线性关系良好,相关系数(r2)均大于0.98;不同基质在10 μg/kg添加水平下大部分农药的平均回收率为66.2%~124.7%,相对标准偏差(RSD)为0.9%~24.4%;方法的定量限(LOQ)为0.03~16.7 μg/kg。结果表明,该方法简便快速、灵敏可靠、经济有效,适用于蔬菜、水果中农药多残留的同时快速筛查测定。 相似文献
19.
固相萃取-三重串联四极杆气相色谱/质谱联用分析蔬菜中43种农药残留留 总被引:4,自引:0,他引:4
建立了气相色谱/三重四极杆串联质谱同时分析蔬菜中43种农药残留的方法。采用乙腈提取样品中待测组分,经固相萃取法(SPE)净化后采用气相色谱/三重四极杆串联质谱在多反应监测(MRM)模式下进行外标法定量测定。分别对青菜进行3个水平(10、80、200 μg/kg)的加标回收试验,其回收率为62.2%~170.0%,其中36种农药的回收率为70.0%~120.0%。方法的相对标准偏差(RSD)小于18%,定量限(LOQ)为0.3~4.4 μg/kg。该分析方法背景干扰低,灵敏度高,适合蔬菜中多种农药及杀虫剂残留的测定。 相似文献
20.
超快速液相色谱-串联质谱法快速筛查蔬菜中176种农药的残留量 总被引:3,自引:0,他引:3
采用超快速液相色谱-串联质谱(UFLC-MS/MS)技术建立了蔬菜中176种农药残留快速筛查的分析方法。蔬菜样品采用乙腈提取,盐析后无需净化。采用多反应监测-信息关联采集-增强子离子扫描(MRM-IDA-EPI)的复合扫描模式,利用基于EPI谱图和色谱峰峰面积的谱库检索技术,完成了蔬菜中176种农药残留的定性定量分析。所有农药在各自的线性范围内线性关系良好(r>0.99),除了丁硫克百威和灭蝇胺在3个添加水平下的平均回收率分别为46.8%和53.1%,其余174种农药的平均回收率范围为72.4%~126.4%,相对标准偏差范围为1.0%~18.7%,方法的检出限和定量限范围分别为0.005~2.0 μg/kg和0.1~10 μg/kg。该方法具有快速、灵敏度高、准确度高等优点,适合于蔬菜样品中农药多残留的快速筛查分析。 相似文献