CN110346459A - 一种分析农药产品中农药隐性成分的lc-ms/ms方法 - Google Patents
一种分析农药产品中农药隐性成分的lc-ms/ms方法 Download PDFInfo
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- CN110346459A CN110346459A CN201810297839.4A CN201810297839A CN110346459A CN 110346459 A CN110346459 A CN 110346459A CN 201810297839 A CN201810297839 A CN 201810297839A CN 110346459 A CN110346459 A CN 110346459A
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- pesticide
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- pesticidal products
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- 238000000034 method Methods 0.000 title claims abstract description 36
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- QNBTYORWCCMPQP-JXAWBTAJSA-N (Z)-dimethomorph Chemical compound C1=C(OC)C(OC)=CC=C1C(\C=1C=CC(Cl)=CC=1)=C/C(=O)N1CCOCC1 QNBTYORWCCMPQP-JXAWBTAJSA-N 0.000 claims 1
- PXMNMQRDXWABCY-UHFFFAOYSA-N 1-(4-chlorophenyl)-4,4-dimethyl-3-(1H-1,2,4-triazol-1-ylmethyl)pentan-3-ol Chemical compound C1=NC=NN1CC(O)(C(C)(C)C)CCC1=CC=C(Cl)C=C1 PXMNMQRDXWABCY-UHFFFAOYSA-N 0.000 claims 1
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- VXMNDQDDWDDKOQ-UHFFFAOYSA-N Pyrazosulfuron Chemical compound COC1=CC(OC)=NC(NC(=O)NS(=O)(=O)C=2N(N=CC=2C(O)=O)C)=N1 VXMNDQDDWDDKOQ-UHFFFAOYSA-N 0.000 claims 1
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- RRZXIRBKKLTSOM-XPNPUAGNSA-N avermectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](O)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 RRZXIRBKKLTSOM-XPNPUAGNSA-N 0.000 claims 1
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- XMQFTWRPUQYINF-UHFFFAOYSA-N bensulfuron-methyl Chemical group COC(=O)C1=CC=CC=C1CS(=O)(=O)NC(=O)NC1=NC(OC)=CC(OC)=N1 XMQFTWRPUQYINF-UHFFFAOYSA-N 0.000 claims 1
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- WOWBFOBYOAGEEA-UHFFFAOYSA-N diafenthiuron Chemical compound CC(C)C1=C(NC(=S)NC(C)(C)C)C(C(C)C)=CC(OC=2C=CC=CC=2)=C1 WOWBFOBYOAGEEA-UHFFFAOYSA-N 0.000 claims 1
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Abstract
一种分析农药产品中农药隐性成分的LC‑MS/MS方法，其特征在于：采用液相色谱‑串联质谱法(LC‑MS/MS)，建立一种农药产品中80种农药隐性成分的精准筛查方法。准确称取适量农药产品，采用乙腈超声提取、稀释处理，过膜后直接进样分析。本发明方法筛查的农药品种覆盖面广、针对性和实用性强，适用于多种不同剂型农药产品，能够准确定性和定量；解决了目前农药隐性成分难于定性定量的难题，可为农药质量监督抽查提供精准检测技术支持。
Description
技术领域：
本发明属于农业投入品安全甄别技术领域，涉及农业投入品中80种高风险、高检出率的农药隐性成分的精准筛查方法，适用于9种剂型农药产品，能满足农药质量安全监督抽检的技术需求。
背景技术：
近年来，随着各级政府部门监管力度的加大，农药市场产品质量不断提升，但假劣农药仍占一定比例，且造假花样不断翻新，一些农药经销商、生产企业代表甚至把添加某些隐性成分作为“卖点”，向农户宣传推荐，对农业生产和农产品质量安全造成严重威胁，必须采取有力措施严厉打击非法添加行为。
农药隐性成分从狭义上讲，指的是在农药制剂中人为添加标称有效成分以外的农药，主要包括：未经登记批准和未过专利保护期的农药以及国家已经禁用的高毒农药。从近年农业部公布的农药监督抽查结果来看，农药产品质量问题主要涉及标称的有效成分未检出、有效成分含量不足及非法添加隐性成分等，其中非法添加隐性成分问题呈逐年增加趋势，并因覆盖面广，检测设备和技术水平等问题而导致实际抽检过程中难于定性定量，是农药监督执法面临的主要难题。
根据中华人民共和国农业部公告中规定的在禁用和限制使用的农药，以及近年来农业部发布的农药产品质量监督抽查结果，本研究确定了80种高风险、高检出率的农药作为研究对象，采用LC-MS/MS法，建立了一种农药产品中农药隐性成分的精准筛查方法。
该方法涉及农药隐性成分种类多、范围广，灵敏度高，能准确定性定量，适用于农药产品质量监管部门的日常监控。
发明内容：
本发明的目的在于解决农药产品非法添加隐性成分现有检测技术水平低、难定性定量的难题，建立一种农药产品中农药隐性成分的精准筛查方法。
本发明的目的是通过以下技术方案来实现的，本发明所述的一种分析农药产品中农药隐性成分的LC-MS/MS方法，包括以下步骤：
a、准确称取农药产品20mg于烧杯中，精确至0.1mg，加入80mL乙腈，超声30min，全部转移至100mL容量瓶，加10mL乙腈清洗烧杯，并转移至容量瓶，冷却至室温，加乙腈定容至100mL，摇匀，此溶液为a液。a液中目标物的浓度在2-200μg/mL范围内。
b、用刻度吸管准确移取a液适量，用乙腈稀释5倍，此溶液为b液。b液中目标物的浓度在0.4-40μg/mL范围内。
c、用刻度吸管准确移取b液适量，用乙腈稀释至约0.1μg/mL，此溶液为c液。
d、吸取c液400μL，加超纯水600μL，混匀，过0.22μm有机滤膜，用LC-MS/MS进样分析。为防止漏检，若通过LC-MS/MS仍未检出时，可将浓度增大至其10倍液复检。
e、准备混合标准工作溶液：用乙腈稀释配制浓度分别为0.005、0.01、0.02、0.05、0.1μg/mL的混合标准工作溶液。
f、采用UPLC-MS/MS法对混合标准溶液和供试样品进行测定，以浓度为横坐标，以定量离子的峰面积为纵坐标绘制标准曲线，计算供试样品中目标农药的含量。
UPLC-MS/MS测定的色谱条件为：色谱柱：AcquityTM BEH RP18柱(2.1×100mm，1.7μm)；流动相：A相为乙腈，B相为0.1％甲酸(含5mmol/L乙酸铵)；梯度洗脱条件见表1。流速：0.2mL/min；进样量：5μL；柱温：40℃。
表1梯度洗脱条件
质谱条件为：电离模式：电喷雾离子源ESI(+,-)；毛细管电压：3.0Kv；离子源温度：150℃；脱溶剂气温度：500℃；脱溶剂气流量：1000L/hr；锥孔反吹气流量：7Bar；检测方式：多反应监测扫描(MRM)；80种农药的保留时间及质谱采集参数见表2。
本发明方法建立了一种分析农药产品中80种高风险农药隐性成分的LC-MS/MS方法，具有简单、快速、能准确定性和定量等优势，灵敏度高，准确度和精密度均符合多残留分析方法的要求。与现有技术相比本发明方法具有以下优良效果。
(1)本发明方法采用UPLC-MS/MS测定，灵敏度高、能准确定性和定量，能满足现行检测技术水平低、难定性定量的需求，目前尚无同类技术报道。
(2)本发明方法筛查的农药品种覆盖面广、针对性强，均属于农业部近年来公布的高风险、高检出率农药隐性成分，能满足实际需要。
(3)本发明方法适用于多种不同农药剂型，包括可湿性粉剂、水分散粒剂、颗粒剂、可溶性粒剂、可溶性粉剂、水剂、悬乳剂、悬浮剂、乳油。
本发明方法的灵敏度：
以信噪比为3计算方法的检测限，80种农药的检测限在0.001～0.01μg/mL之间。
本发明方法的线性：
以各组分的浓度为横坐标，色谱峰面积为纵坐标，绘制标准曲线。90种目标农药在0.001～0.1μg/mL浓度范围内，浓度与峰面积呈良好的线性关系，相关系数在0.991～0.999之间。
本发明方法的准确度和精密度：
对9种剂型农药产品进行了加标回收率试验，包括50％呋虫胺水分散粒剂、10％吡虫啉可湿性粉剂、6％毒死蜱·辛硫磷颗粒剂、40％赤霉酸可溶粒剂、0.004％芸苔素内酯水剂、42％异丙甲草胺·嗪草酮悬乳剂、25％氯虫苯甲酰胺·啶虫脒可分散油悬浮剂、620g/L莠去津-苯唑草酮悬浮剂、47.5g/L+475g/L氯氰菊酯·毒死蜱乳油，在已知含量的试样中添加一定量的目标物混合标准溶液，在上述色谱和质谱条件下进行测定，重复5次，结果表明各组分平均回收率在93％～101％之间，相对标准偏差小于6.8％，准确度和精密度均符合分析方法要求。
表2 80种农药的保留时间、质谱采集参数、标准曲线、相关系数和灵敏度
具体实施方式
下面结合实施例对本发明做进一步的说明，实施例仅为解释性的，决不意味着它以任何方式限制本发明的范围。
实施例1
以供试10％吡虫啉可湿性粉剂为样本，采用本发明方法进行样品前处理，采用超高效液相色谱-串联质谱法测定。制备方法如下：
1、仪器与试剂
美国Waters超高效液相色谱-串联质谱仪I-Class/Xevo TQ-S三重四极杆质谱仪；瑞士Mettler感量0.00001g电子天平；超声萃取仪；农药标准品纯度均不低于99％，购自德国Dr.E公司；乙腈、甲酸为色谱纯。
2、样品前处理方法
a、准确称取农药产品20mg于烧杯中，精确至0.1mg，加入80mL乙腈，超声30min，全部转移至100mL容量瓶，加10mL乙腈清洗烧杯，并转移至容量瓶，冷却至室温，加乙腈定容至100mL，摇匀，此溶液为a液。a液中吡虫啉的浓度为20μg/mL。
b、用刻度吸管准确移取a液适量，用乙腈稀释5倍，此溶液为b液。b液中吡虫啉的浓度为4μg/mL。
c、用刻度吸管准确移取b液适量，用乙腈稀释40倍，此溶液为c液。c液中吡虫啉的浓度为0.1μg/mL。
d、吸取c液400μL，加超纯水600μL，混匀，过0.22μm有机滤膜，用LC-MS/MS进样分析。
3、准备标准工作溶液
用乙腈稀释配制浓度分别为0.005、0.01、0.02、0.05、0.1μg/mL的混合标准工作溶液。
4、测定方法
UPLC-MS/MS测定的色谱条件为：色谱柱：AcquityTM BEH RP18柱(2.1×100mm，1.7μm)；流动相：乙腈-0.1％甲酸(含5mmol/L乙酸铵)；梯度洗脱条件见表1。流速：0.2mL/min；进样量：5μL；柱温：40℃。
质谱条件为：电离模式：电喷雾离子源ESI(+,-)；毛细管电压：3.0Kv；离子源温度：150℃；脱溶剂气温度：500℃；脱溶剂气流量：1000L/hr；锥孔反吹气流量：7Bar；检测方式：多反应监测扫描(MRM)；80种农药的保留时间及质谱采集参数见表2。
5、结果计算
采用UPLC-MS/MS法对系列浓度的混合标准溶液和供试样品进行测定，以浓度为横坐标，定量离子的峰面积为纵坐标，绘制标准曲线，计算供试样品中目标农药的含量。计算结果见表3。
计算公式：
其中：
ω-农药隐性成分含量(％)
C0-根据标准曲线计算的样品溶液中目标物的浓度(μg/mL)
稀释倍数-b液稀释至c液的稀释倍数
6、农药隐性成分测定结果
结果显示，在实测样品10％吡虫啉可湿性粉剂中，检出禁用高毒农药克百威，含量2％。
Claims (4)
1.一种分析农药产品中农药隐性成分的LC-MS/MS方法，其特征在于：采用液相色谱-串联质谱法(LC-MS/MS)，建立一种农药产品中80种农药隐性成分的精准筛查方法。准确称取适量农药产品，采用乙腈超声提取、稀释处理，针筒过滤后直接进样分析。本发明方法解决了目前农药隐性成分难于定性定量的难题，可为农药质量监督抽查提供精准检测技术支持。
具体步骤如下：
a、准确称取农药产品20mg于烧杯中，精确至0.1mg，加入80mL乙腈，超声30min，全部转移至100mL容量瓶，加10mL乙腈清洗烧杯，并转移至容量瓶，冷却至室温，加乙腈定容至100mL，摇匀，此溶液为a液。a液中目标物的浓度在2-200μg/mL范围内。
b、用刻度吸管准确移取a液适量，用乙腈稀释5倍，此溶液为b液。b液中目标物的浓度在0.4-40μg/mL范围内。
c、用刻度吸管准确移取b液适量，用乙腈稀释至约0.1μg/mL，此溶液为c液。
d、吸取c液400μL，加超纯水600μL，混匀，过0.22μm有机滤膜，用LC-MS/MS进样分析。为防止漏检，若通过LC-MS/MS仍未检出时，可将浓度增大至其10倍液复检。
e、准备标准储备溶液：分别称取各农药标准品适量，用乙腈溶解，配制浓度为200μg/mL的农药标准储备溶液。
f、准备混合标准溶液：分别取适量标准储备溶液，用乙腈稀释并定容，配制浓度为10μg/mL的混合标准溶液，用乙腈稀释配制浓度分别为0.005、0.01、0.02、0.05、0.1μg/mL的混合标准工作溶液。
g、采用LC-MS/MS法对混合标准工作溶液和供试样品进行测定，以浓度为横坐标，定量离子的峰面积为纵坐标绘制标准曲线，以此标准曲线来计算供试样品中目标物的含量。
2.权利要求1所述的分析农药产品中农药隐性成分的LC-MS/MS方法，其中的农药产品剂型为可湿性粉剂、水分散粒剂、颗粒剂、可溶性粒剂、可溶性粉剂、水剂、悬乳剂、悬浮剂、乳油。
3.权利要求1所述的分析农药产品中农药隐性成分的LC-MS/MS方法，其中80种农药隐性成分是甲胺磷、久效磷、磷胺、杀扑磷、水胺硫磷、灭线磷、马拉硫磷、三唑磷、氯唑磷、甲基异柳磷、地虫硫磷、治螟磷、蝇毒磷、甲拌磷、辛硫磷、特丁硫磷、毒死蜱、氧化乐果、苯线磷、内吸磷、硫环磷、敌敌畏、灭多威、抗蚜威、速灭威、克百威、丁硫克百威、涕灭威、异丙威、仲丁威、乙霉威、茚虫威、噻虫嗪、敌百虫、吡虫啉、啶虫脒、吡丙醚、吡蚜酮、噻嗪酮、氟虫腈、氟铃脲、阿维菌素、杀虫脒、氯虫苯甲酰胺、烯啶虫胺、丁醚脲、哒螨灵、螺螨酯、多菌灵、甲基硫菌灵、嘧霉胺、甲霜灵、福美双、甲基阿维菌素苯甲酸盐、烯酰吗啉、腈菌唑、三唑酮、嘧菌酯、戊唑醇、己唑醇、苯醚甲环唑、西草净、莠去津、异恶草酮、甲草胺、乙草胺、硝磺草酮、双氟磺草胺、甲磺隆、氯磺隆、苯磺隆、烟嘧磺隆、苄嘧磺隆、氯嘧磺隆、吡嘧磺隆、矮壮素、氯吡脲、多效唑、2,4-D、噻苯隆。
4.权利要求1所述的分析农药产品中农药隐性成分的LC-MS/MS方法，采用的色谱条件为：C18反相色谱柱，流动相由有机相和水相组成，有机相是乙腈，水相是0.1％甲酸水溶液，甲酸水溶液含有5mmol/L乙酸铵，采用梯度洗脱，流速0.2mL/min，柱温40℃，进样体积5μL。采用的质谱条件为：电喷雾电离，多反应监测扫描，正离子毛细管电压3.0kv，负离子毛细管电压2.0kv，离子源温度150℃，脱溶剂气温度450℃，脱溶剂气流量900L/hr，锥孔电压10-90V，碰撞能量10-90V。
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111948317A (zh) * | 2020-08-14 | 2020-11-17 | 江苏省农产品质量检验测试中心 | 一种氟铃脲的高效液相色谱分析方法 |
| CN112697891A (zh) * | 2020-11-05 | 2021-04-23 | 广电计量检测(南宁)有限公司 | 一种桑叶中超微量吡丙醚的检测方法 |
| CN112946097A (zh) * | 2021-01-19 | 2021-06-11 | 中国农业科学院茶叶研究所 | 一种茶叶和茶汤中螺螨酯残留分析测定方法 |
| CN114236009A (zh) * | 2021-12-17 | 2022-03-25 | 中国农业科学院农业质量标准与检测技术研究所 | 一种农药制剂中隐性违禁添加化学品的筛查方法 |
| CN115097047A (zh) * | 2022-07-15 | 2022-09-23 | 浙江省产品质量安全科学研究院 | 驱蚊产品中农药含量测定的液相色谱-串联质谱方法 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1962087A1 (en) * | 2005-12-12 | 2008-08-27 | Universidad de Castilla-La Mancha | Gas chromatography system and method |
| US20080234158A1 (en) * | 2007-03-22 | 2008-09-25 | Jih Ru Hwu | Compositions counteracting pesticides and malodorants |
| CN104374859A (zh) * | 2014-11-25 | 2015-02-25 | 苏州东辰林达检测技术有限公司 | 一种紫甘蓝中有机磷农药残留的检测方法 |
| CN106596821A (zh) * | 2016-12-12 | 2017-04-26 | 中国测试技术研究院 | 一种农药制剂中有机溶剂的快速测定方法 |
| CN107478737A (zh) * | 2017-07-18 | 2017-12-15 | 贵州茅台酒股份有限公司 | 一种检测白酒中80种农药残留量的方法 |
-
2018
- 2018-04-04 CN CN201810297839.4A patent/CN110346459A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1962087A1 (en) * | 2005-12-12 | 2008-08-27 | Universidad de Castilla-La Mancha | Gas chromatography system and method |
| US20080234158A1 (en) * | 2007-03-22 | 2008-09-25 | Jih Ru Hwu | Compositions counteracting pesticides and malodorants |
| CN104374859A (zh) * | 2014-11-25 | 2015-02-25 | 苏州东辰林达检测技术有限公司 | 一种紫甘蓝中有机磷农药残留的检测方法 |
| CN106596821A (zh) * | 2016-12-12 | 2017-04-26 | 中国测试技术研究院 | 一种农药制剂中有机溶剂的快速测定方法 |
| CN107478737A (zh) * | 2017-07-18 | 2017-12-15 | 贵州茅台酒股份有限公司 | 一种检测白酒中80种农药残留量的方法 |
Non-Patent Citations (3)
| Title |
|---|
| 乔成奎等: "HPLC-MS/MS 法检测农药产品中30 种隐性成分", 《农药》 * |
| 于峰等: "建立HPLC-DAD-MS/MS 指纹图谱快速分析农药隐性成分的方法", 《农药》 * |
| 崔勇等: "生活饮用水及水源水中15种有机污染物残留量的超高效液相色谱-串联质谱同时测定法", 《环境与健康杂志》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111948317A (zh) * | 2020-08-14 | 2020-11-17 | 江苏省农产品质量检验测试中心 | 一种氟铃脲的高效液相色谱分析方法 |
| CN112697891A (zh) * | 2020-11-05 | 2021-04-23 | 广电计量检测(南宁)有限公司 | 一种桑叶中超微量吡丙醚的检测方法 |
| CN112946097A (zh) * | 2021-01-19 | 2021-06-11 | 中国农业科学院茶叶研究所 | 一种茶叶和茶汤中螺螨酯残留分析测定方法 |
| CN114236009A (zh) * | 2021-12-17 | 2022-03-25 | 中国农业科学院农业质量标准与检测技术研究所 | 一种农药制剂中隐性违禁添加化学品的筛查方法 |
| CN115097047A (zh) * | 2022-07-15 | 2022-09-23 | 浙江省产品质量安全科学研究院 | 驱蚊产品中农药含量测定的液相色谱-串联质谱方法 |
| CN115097047B (zh) * | 2022-07-15 | 2023-08-22 | 浙江省产品质量安全科学研究院 | 驱蚊产品中农药含量测定的液相色谱-串联质谱方法 |
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