全自动QuEChERS前处理仪结合气相色谱-四极杆-飞行时间质谱法测定橄榄油中222种农药残留
O658; 基于QuEChERS方法,建立了全自动 QuEChERS 前处理仪结合气相色谱-四极杆-飞行时间质谱法(GC-QTOF-MS)快速测定橄榄油中222 种农药残留的分析方法,并考察了提取溶剂酸化程度、正己烷体积、振荡时间、离心温度、净化剂对 222 种农药残留测定的影响.首先选择响应较好且无明显干扰的离子用于定量及定性,再通过对全自动QuEChERS前处理仪的参数设置开发了净化流程,用含 2%甲酸的乙腈溶液提取,上清液在含有 400 mg N-丙基乙二胺(PSA)、400 mg十八烷基硅烷键合硅胶(C18)和1 200 mg无水硫酸镁的离心管中净化离心,净化液经氮气吹干,用乙酸乙酯定...
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| Published in | Sepu Vol. 42; no. 4; pp. 368 - 379 |
|---|---|
| Main Authors | , , , , , , , |
| Format | Journal Article |
| Language | Chinese English |
| Published |
No. 457, Zhongshan Road, Shahekou District, Dalian City, Liaoning Province
甘肃农业大学食品科学与工程学院,甘肃 兰州 730070%兰州海关技术中心,甘肃 兰州 730010%甘肃农业大学食品科学与工程学院,甘肃 兰州 730070
08.04.2024
兰州海关技术中心,甘肃 兰州 730010%西北师范大学地理与环境科学学院,甘肃 兰州 730070 Editorial board of Chinese Journal of Chromatography |
| Subjects | |
| Online Access | Get full text |
| ISSN | 1000-8713 1872-2059 |
| DOI | 10.3724/SP.J.1123.2023.09010 |
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| Abstract | O658; 基于QuEChERS方法,建立了全自动 QuEChERS 前处理仪结合气相色谱-四极杆-飞行时间质谱法(GC-QTOF-MS)快速测定橄榄油中222 种农药残留的分析方法,并考察了提取溶剂酸化程度、正己烷体积、振荡时间、离心温度、净化剂对 222 种农药残留测定的影响.首先选择响应较好且无明显干扰的离子用于定量及定性,再通过对全自动QuEChERS前处理仪的参数设置开发了净化流程,用含 2%甲酸的乙腈溶液提取,上清液在含有 400 mg N-丙基乙二胺(PSA)、400 mg十八烷基硅烷键合硅胶(C18)和1 200 mg无水硫酸镁的离心管中净化离心,净化液经氮气吹干,用乙酸乙酯定容后供仪器分析,最后采用基质标准溶液进行定量.从基质效应、线性范围、检出限、定量限、精密度及正确度等方面对定量分析方法进行验证.结果表明:222 种农药中 86.04%的农药线性范围为 0.02～2.00 μg/mL,10.81%农药的线性范围为0.10～2.00 μg/mL,3.15%农药的线性范围为0.20～2.00 μg/mL,相关系数(R2)均大于 0.99,222 种农药在各自线性范围内线性关系良好;全部被测农药的检出限范围为 0.002～0.050 mg/kg,定量限范围为 0.007～0.167 mg/kg,其中有 170 种农药定量限可以达到 0.007 mg/kg,21 种农药定量限可以达到 0.017 mg/kg,占总数量的 86.04%;在 0.2、0.5 和 0.8 mg/kg 3 个添加水平下,平均回收率为 70%～120%的农药占全部被测农药的 79.58%,平均回收率为 80%～110%的农药占全部被测农药的 65.92%,相对标准偏差(RSD,n=6)＜10%的农药占全部被测农药的 93.54%,RSD(n=6)＜20%的农药占全部被测农药的 98.35%.应用该方法对 14 份市售橄榄油样品进行了检测,共检出 7 种农药,其含量范围为 0.0044～0.0490 mg/kg.该方法操作简单、快速、灵敏度高,且自动化程度较强,前处理过程无需人员值守,减轻劳动力的同时减少了人员误差,能够满足橄榄油中多种农药残留检测的需求,也可以为其他油类农药残留检测及复杂基质的自动化前处理提供参考. |
|---|---|
| AbstractList | 基于QuEChERS方法,建立了全自动QuEChERS前处理仪结合气相色谱-四极杆-飞行时间质谱法(GC-QTOF-MS)快速测定橄榄油中222种农药残留的分析方法,并考察了提取溶剂酸化程度、正己烷体积、振荡时间、离心温度、净化剂对222种农药残留测定的影响。首先选择响应较好且无明显干扰的离子用于定量及定性,再通过对全自动QuEChERS前处理仪的参数设置开发了净化流程,用含2%甲酸的乙腈溶液提取,上清液在含有400 mg
N
-丙基乙二胺(PSA)、400 mg十八烷基硅烷键合硅胶(C18)和1 200 mg无水硫酸镁的离心管中净化离心,净化液经氮气吹干,用乙酸乙酯定容后供仪器分析,最后采用基质标准溶液进行定量。从基质效应、线性范围、检出限、定量限、精密度及正确度等方面对定量分析方法进行验证。结果表明:222种农药中86.04%的农药线性范围为0.02~2.00 μg/mL, 10.81%农药的线性范围为0.10~2.00 μg/mL, 3.15%农药的线性范围为0.20~2.00 μg/mL,相关系数(
R
2
)均大于0.99,222种农药在各自线性范围内线性关系良好;全部被测农药的检出限范围为0.002~0.050 mg/kg,定量限范围为0.007~0.167 mg/kg,其中有170种农药定量限可以达到0.007 mg/kg, 21种农药定量限可以达到0.017 mg/kg,占总数量的86.04%;在0.2、0.5和0.8 mg/kg 3个添加水平下,平均回收率为70%~120%的农药占全部被测农药的79.58%,平均回收率为80%~110%的农药占全部被测农药的65.92%,相对标准偏差(RSD,
n
=6)<10%的农药占全部被测农药的93.54%, RSD(
n
=6)<20%的农药占全部被测农药的98.35%。应用该方法对14份市售橄榄油样品进行了检测,共检出7种农药,其含量范围为0.0044~0.0490 mg/kg。该方法操作简单、快速、灵敏度高,且自动化程度较强,前处理过程无需人员值守,减轻劳动力的同时减少了人员误差,能够满足橄榄油中多种农药残留检测的需求,也可以为其他油类农药残留检测及复杂基质的自动化前处理提供参考。 O658; 基于QuEChERS方法,建立了全自动 QuEChERS 前处理仪结合气相色谱-四极杆-飞行时间质谱法(GC-QTOF-MS)快速测定橄榄油中222 种农药残留的分析方法,并考察了提取溶剂酸化程度、正己烷体积、振荡时间、离心温度、净化剂对 222 种农药残留测定的影响.首先选择响应较好且无明显干扰的离子用于定量及定性,再通过对全自动QuEChERS前处理仪的参数设置开发了净化流程,用含 2%甲酸的乙腈溶液提取,上清液在含有 400 mg N-丙基乙二胺(PSA)、400 mg十八烷基硅烷键合硅胶(C18)和1 200 mg无水硫酸镁的离心管中净化离心,净化液经氮气吹干,用乙酸乙酯定容后供仪器分析,最后采用基质标准溶液进行定量.从基质效应、线性范围、检出限、定量限、精密度及正确度等方面对定量分析方法进行验证.结果表明:222 种农药中 86.04%的农药线性范围为 0.02～2.00 μg/mL,10.81%农药的线性范围为0.10～2.00 μg/mL,3.15%农药的线性范围为0.20～2.00 μg/mL,相关系数(R2)均大于 0.99,222 种农药在各自线性范围内线性关系良好;全部被测农药的检出限范围为 0.002～0.050 mg/kg,定量限范围为 0.007～0.167 mg/kg,其中有 170 种农药定量限可以达到 0.007 mg/kg,21 种农药定量限可以达到 0.017 mg/kg,占总数量的 86.04%;在 0.2、0.5 和 0.8 mg/kg 3 个添加水平下,平均回收率为 70%～120%的农药占全部被测农药的 79.58%,平均回收率为 80%～110%的农药占全部被测农药的 65.92%,相对标准偏差(RSD,n=6)＜10%的农药占全部被测农药的 93.54%,RSD(n=6)＜20%的农药占全部被测农药的 98.35%.应用该方法对 14 份市售橄榄油样品进行了检测,共检出 7 种农药,其含量范围为 0.0044～0.0490 mg/kg.该方法操作简单、快速、灵敏度高,且自动化程度较强,前处理过程无需人员值守,减轻劳动力的同时减少了人员误差,能够满足橄榄油中多种农药残留检测的需求,也可以为其他油类农药残留检测及复杂基质的自动化前处理提供参考. |
| Abstract_FL | Pesticide residues may be present in olive oil because pesticides are applied to olive trees during their cultivation and growth for pest prevention and some of these pesticides are not easily degraded.Studies on pesticide residues in olive oil have mainly focused on the detec-tion of single types of pesticide residues,and reports on the simultaneous detection of multiple pesticide residues are limited.At present,hundreds of pesticides with different polarities and chemical properties are used in practice.
In this study,an analytical method based on fully automatic QuEChERS pretreatment instru-ment coupled with gas chromatography-quadrupole time-of-flight mass spectrometry(GC-QTOF-MS)was established for the rapid determination of 222 pesticide residues in olive oil.The effects of acetonitrile acidification concentration,n-hexane volume,oscillation time,cen-trifugation temperature,and purification agent on the determination of the 222 pesticide resi-dues were investigated.First,ions with good responses and no obvious interference were se-lected for quantification and characterization.The purification process was then developed by setting the parameters of the fully automatic QuEChERS pretreatment instrument to optimal val-ues.The sample was extracted with acetonitrile containing 2%formic acid,and the supernatant was purified by centrifugation in a centrifuge tube containing 400 mg N-propylethylenediamine(PSA),400 mg octadecylsilane-bonded silica gel(C18),and 1 200 mg anhydrous magnesium sulfate.The purified solution was blown dry with nitrogen and then fixed with ethyl acetate for instrumental analysis.Finally,a matrix standard solution was used for quantification.The meth-od was validated in terms of matrix effects,linear ranges,limits of detection(LODs)and quantification(LOQs),accuracies,and precisions.The results showed that 86.04%of the 222 pesticides had linear ranges of 0.02-2.00 μg/mL,10.81%had linear ranges of 0.10-2.00 μg/mL,and 3.15%had linear ranges of 0.20-2.00 μg/mL.The pesticide residues showed good relationships within their respective linear ranges,and the correlation coefficients(R2)were greater than 0.99.The LODs of all tested pesticides ranged from 0.002 to 0.050 mg/kg,and their LOQs ranged from 0.007 to 0.167 mg/kg.Among the 222 pesticides determined,170 pesti-cides had LOQs of 0.007 mg/kg while 21 pesticides had LOQs of 0.017 mg/kg.At the three spiked levels of 0.2,0.5,and 0.8 mg/kg,79.58%of all tested pesticides had average recover-ies of 70%-120%while 65.92%had average recoveries of 80%-110%.In addition,93.54%of all tested pesticides had relative standard deviations(RSDs,n=6)＜10%while 98.35%had RSDs(n=6)＜20%.The method was applied to 14 commercially available olive oil samples,and seven pesticides were detected in the range of 0.0044-0.0490 mg/kg.The residues of fenbuconazole,chlorpyrifos,and methoprene did not exceed the maximum limits stated in GB 2763-2021.The maximum residual limits of molinate,monolinuron,benalaxyl,and thiobencarb have not been established.The method utilizes the high mass resolution capability of TOF-MS,which can im-prove the detection throughput while ensuring good sensitivity.In addition,high-resolution and accurate mass measurements render the screening results more reliable,which is necessary for the high-throughput detection of pesticide residues.The use of a fully automatic QuEChERS in-strument in the pretreatment step reduces personnel errors and labor costs,especially when a large number of samples must be processed,thereby offering significant advantages over other approaches.Moreover,the method is simple,rapid,sensitive,highly automatable,accurate,and precise.Thus,it meets requirements for the high-throughput detection of pesticide residues in olive oil and provides a reference for the development of detection methods for pesticide resi-dues in other types of oils as well as the automatic pretreatment of complex matrices. |
| Author | 雷春妮 朱梦晨 周小平 王新潮 王波 张欢 漆珍珍 梁艳 |
| AuthorAffiliation | 甘肃农业大学食品科学与工程学院,甘肃 兰州 730070%兰州海关技术中心,甘肃 兰州 730010%甘肃农业大学食品科学与工程学院,甘肃 兰州 730070;兰州海关技术中心,甘肃 兰州 730010%西北师范大学地理与环境科学学院,甘肃 兰州 730070 |
| AuthorAffiliation_xml | – name: 甘肃农业大学食品科学与工程学院,甘肃 兰州 730070%兰州海关技术中心,甘肃 兰州 730010%甘肃农业大学食品科学与工程学院,甘肃 兰州 730070;兰州海关技术中心,甘肃 兰州 730010%西北师范大学地理与环境科学学院,甘肃 兰州 730070 |
| Author_FL | LEI Chunni QI Zhenzhen ZHOU Xiaoping WANG Xinchao LIANG Yan ZHU Mengchen ZHANG Huan WANG Bo |
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| Author_xml | – sequence: 1 fullname: 梁艳 – sequence: 2 fullname: 雷春妮 – sequence: 3 fullname: 王波 – sequence: 4 fullname: 张欢 – sequence: 5 fullname: 王新潮 – sequence: 6 fullname: 周小平 – sequence: 7 fullname: 漆珍珍 – sequence: 8 fullname: 朱梦晨 |
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| DocumentTitle_FL | Determination of 222 pesticide residues in olive oil by fully automatic QuEChERS pre-treatment instrument coupled with gas chromatography-quadrupole-time-of-flight mass spectrometry |
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| Keywords | 全自动QuEChERS前处理仪 农药残留 橄榄油 气相色谱-四极杆-飞行时间质谱 fully automatic QuEChERS pre-treatment instrument pesticide residues olive oil gas chromatography-quadru-pole-time-of-flight mass spectrometry(GC-QTOF-MS) |
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| Publisher | 甘肃农业大学食品科学与工程学院,甘肃 兰州 730070%兰州海关技术中心,甘肃 兰州 730010%甘肃农业大学食品科学与工程学院,甘肃 兰州 730070 兰州海关技术中心,甘肃 兰州 730010%西北师范大学地理与环境科学学院,甘肃 兰州 730070 Editorial board of Chinese Journal of Chromatography |
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| Title | 全自动QuEChERS前处理仪结合气相色谱-四极杆-飞行时间质谱法测定橄榄油中222种农药残留 |
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