方案摘要
方案下载应用领域 | 农/林/牧/渔 |
检测样本 | 生物农药 |
检测项目 | |
参考标准 | GB 23200.113-2018 |
本文参考《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》标准(GB 23200.113-2018),使用气相色谱-串联三重四极杆质谱联用仪对黄瓜基质中的113多种农药及相关化学品进行检测分析,通过定量限、精密度和准确度等指标评估仪器性能,证明GC-TQ 6000满足检测的需要。
前言
农药是农业上用于防治病虫害及调节植物生长的化学试剂,广泛用于农林牧业生产、环境和家庭卫生除害防疫、工业品防霉和防蛀等。农药的大量使用容易会导致其在食物链及环境中残留,对人类健康和生态环境造成潜在的危害。因此,建立各类果蔬中农药残留的准确定性定量方法,为老百姓食品安全提供重要保障。
本文参考《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》标准(GB 23200.113-2018),使用气相色谱-串联三重四极杆质谱联用仪对黄瓜基质中的107多种农药及相关化学品进行检测分析,通过定量限、精密度和准确度等指标评估仪器性能,证明GC-TQ 6000满足检测的需要。
实验部分
样品前处理
准确称取10 g黄瓜样品于50 mL离心管中,加入10 mL乙腈和1包QuEChERS萃取盐包,盖上离心管,剧烈振荡3 min后4200 r/min离心5 min。吸取6 mL上清液加到内含净化盐包的15 mL离心管中,涡旋混匀2 min。4200 r/min离心5 min,准确吸取2 mL上清液于10 mL试管中,40℃水浴氮吹近干。加入10 μL内标溶液,1mL乙酸乙酯溶液复溶,过0.22 μm有机滤膜,待测。
仪器条件
表1. 仪器方法参数
模块 | 参数 | 值 |
色谱 | 进样口温度 | 280 °C |
进样方式 | 不分流 | |
色谱柱 | VF-1701MS, 30 m × 0.25 mm × 0.25 μm | |
升温程序 | 起始温度40°C,保持1 min,以40°C/min升至120 °C,再以5 °C/min升至240 °C,再以12℃/min升至300℃,保持6min | |
载气 | 氦气 | |
柱流量 | 1.0 mL/min 恒流模式 | |
质谱 | 离子源 | EI,70eV |
离子源温度 | 280 °C | |
传输线温度 | 280 °C | |
检测器电压 | -1300 V | |
溶剂延迟 碰撞气流量 射出电压(CXP) | 4min 20psi 3V | |
采集模式 | MRM |
结果与讨论
1、标准谱图和物质信息
实验总离子流图见图1,107种农药目标化合物浓度为500 μg/L,内标物浓度为100 μg/L。107种目标化合物以及内标的保留时间以及特征离子信息见附录表3。
图1 107种农药目标化合物总离子流图(500 μg/L)
2、标准曲线
黄瓜空白基质溶液氮吹近干,分别加入1 mL浓度为5 μg/L、10 μg/L、20 μg/L、50 μg/L、100 μg/L、200 μg/L、500 μg/L,内标含量为100 μg/L的混合标准曲线溶液进行分析。107种农药的线性相关系数R均大于0.995。
| ||
(a) 敌敌畏 | (b) 一溴二氯甲烷 | (c) 啶酰菌胺 |
图2 三种代表性农药目标化合物的标准曲线图
3、黄瓜加标回收实验
3.1 精密度和准确度
分别对10g黄瓜样品进行加标浓度为0.01 mg/kg、0.05 mg/kg、0.1 mg/kg各六次平行实验,对精密度和准确度进行评估,准确度具体信息详见附录表4。浓度为0.01 mg/kg、0.05 mg/kg和0.1 mg/kg时,107种农药化合物的相对标准偏差(RSD)分别为1.90%-14.54%、1.43%-9.32%和1.00%-4.81%,回收率分别为65.8%-121.2%、66.0%-117.8%、67.2%-113.3%。
3.2 定量限
按照标准GB/T 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》对10g黄瓜进行加标量为0.01 mg/kg的7次平行回收实验,计算其标准偏差(SD),根据方法定量限LOQ=10×SD计算目标化合物的方法定量限,通过计算可知107种农药化合物的方法定量限为0.001 mg/kg-0.010 mg/kg。
表2.107种农药化合物黄瓜基质加标方法定量限
序号 | 化合物 | 方法 定量限(mg/kg) | 标准要求 方法定量限(mg/kg) | 序号 | 化合物 | 方法 定量限(mg/kg) | 标准要求 方法定量限(mg/kg) | |
1 | 敌敌畏 | 0.010 | 0.01 | 55 | 4,4'-滴滴伊 | 0.003 | 0.01 | |
2 | 甲胺磷 | 0.002 | 0.01 | 56 | 苯硫威 | 0.002 | 0.01 | |
3 | 敌草腈 | 0.010 | 0.01 | 57 | 嘧菌胺 | 0.003 | 0.01 | |
4 | 速灭磷 | 0.006 | 0.01 | 58 | 脱叶磷 | 0.010 | 0.01 | |
5 | 虫螨畏 | 0.005 | 0.01 | 59 | 甲拌磷砜 | 0.002 | 0.01 | |
6 | 禾草敌 | 0.010 | 0.01 | 60 | 除草定 | 0.005 | 0.01 | |
7 | 环草敌 | 0.003 | 0.01 | 61 | 三唑醇 | 0.005 | 0.01 | |
8 | 异丙威 | 0.003 | 0.01 | 62 | 溴苯烯磷 | 0.003 | 0.01 | |
9 | 乙酰甲胺磷 | 0.003 | 0.01 | 63 | 丙草胺 | 0.003 | 0.01 | |
10 | 六氯苯 | 0.006 | 0.01 | 64 | 2,4'-滴滴滴 | 0.004 | 0.01 | |
11 | 灭线磷 | 0.003 | 0.01 | 65 | 醚菌酯 | 0.010 | 0.01 | |
12 | 乙丁烯氟灵 | 0.002 | 0.01 | 66 | 异狄氏剂 | 0.010 | 0.01 | |
13 | 残杀威 | 0.003 | 0.01 | 67 | 灭菌磷 | 0.002 | 0.01 | |
14 | 治螟磷 | 0.003 | 0.01 | 68 | 噁草酮 | 0.003 | 0.01 | |
15 | α-六六六 | 0.004 | 0.01 | 69 | 2,4-滴滴涕 | 0.002 | 0.01 | |
16 | 脱乙基莠去津 | 0.004 | 0.01 | 70 | 抑霉唑 | 0.005 | 0.01 | |
17 | 特丁硫磷 | 0.002 | 0.01 | 71 | 地胺磷 | 0.002 | 0.01 | |
18 | 敌噁磷 | 0.006 | 0.01 | 72 | 环氟菌胺 | 0.010 | 0.01 | |
19 | 野麦畏 | 0.002 | 0.01 | 73 | 虫螨磷 | 0.005 | 0.01 | |
20 | 环丙氟灵 | 0.005 | 0.01 | 74 | 乙嘧酚磺酸酯 | 0.004 | 0.01 | |
21 | 地虫硫磷 | 0.003 | 0.01 | 75 | 乙氧氟草醚 | 0.004 | 0.01 | |
22 | 丁基嘧啶磷 | 0.002 | 0.01 | 76 | 噁唑啉 | 0.004 | 0.01 | |
23 | 扑灭津 | 0.003 | 0.01 | 77 | 氟酰胺 | 0.003 | 0.01 | |
24 | 氯硝胺 | 0.004 | 0.01 | 78 | 4,4'-滴滴滴 | 0.003 | 0.01 | |
25 | 胺丙畏 | 0.003 | 0.01 | 79 | β-硫丹 | 0.006 | 0.01 | |
26 | 异稻瘟净 | 0.010 | 0.01 | 80 | 喹氧灵 | 0.002 | 0.01 | |
27 | 除线磷 | 0.002 | 0.01 | 81 | 苯草醚 | 0.002 | 0.01 | |
28 | 抗蚜威 | 0.003 | 0.01 | 82 | 肟菌酯 | 0.004 | 0.01 | |
29 | 久效磷 | 0.003 | 0.01 | 83 | 三硫磷 | 0.005 | 0.01 | |
30 | 乐果 | 0.007 | 0.01 | 84 | 增效醚 | 0.004 | 0.01 | |
31 | 乙草胺 | 0.004 | 0.01 | 85 | 敌瘟磷 | 0.002 | 0.01 | |
32 | 甲草胺 | 0.003 | 0.01 | 86 | 丰索磷 | 0.004 | 0.01 | |
33 | 甲基嘧啶磷 | 0.004 | 0.01 | 87 | 联苯菊酯 | 0.003 | 0.01 | |
34 | 甲基对氧磷 | 0.004 | 0.01 | 88 | 三唑磷 | 0.005 | 0.01 | |
35 | 乙烯菌核利 | 0.004 | 0.01 | 89 | 吡螨胺 | 0.002 | 0.01 | |
36 | 嗪草酮 | 0.002 | 0.01 | 90 | 溴螨酯 | 0.002 | 0.01 | |
37 | 甲霜灵 | 0.009 | 0.01 | 91 | 胺菊酯 | 0.009 | 0.01 | |
38 | 禾草丹 | 0.009 | 0.01 | 92 | 氟环唑 | 0.003 | 0.01 | |
39 | 异丙甲草胺 | 0.010 | 0.01 | 93 | 戊唑醇 | 0.004 | 0.01 | |
40 | 安硫磷 | 0.005 | 0.01 | 94 | 吡丙醚 | 0.005 | 0.01 | |
41 | 三氯杀螨醇 | 0.005 | 0.01 | 95 | 哌草磷 | 0.004 | 0.01 | |
42 | 倍硫磷 | 0.003 | 0.01 | 96 | 苯硫磷 | 0.009 | 0.01 | |
43 | 溴硫磷 | 0.004 | 0.01 | 97 | 环嗪酮 | 0.002 | 0.01 | |
44 | 对氧磷 | 0.010 | 0.01 | 98 | 咪唑菌酮 | 0.003 | 0.01 | |
45 | 三唑酮 | 0.006 | 0.01 | 99 | 三氯杀螨砜 | 0.010 | 0.01 | |
46 | 烯丙菊酯 | 0.007 | 0.01 | 100 | 莎稗磷 | 0.006 | 0.01 | |
47 | 对硫磷 | 0.005 | 0.01 | 101 | 氯菊酯 | 0.005 | 0.01 | |
48 | 甲基异柳磷 | 0.001 | 0.01 | 102 | 氯苯嘧啶醇 | 0.004 | 0.01 | |
49 | 异柳磷 | 0.005 | 0.01 | 103 | 哒螨灵 | 0.008 | 0.01 | |
50 | α-硫丹 | 0.010 | 0.01 | 104 | 氯氰菊酯 | 0.009 | 0.01 | |
51 | 喹硫磷 | 0.002 | 0.01 | 105 | 啶酰菌胺 | 0.003 | 0.01 | |
52 | 戊菌唑 | 0.003 | 0.01 | 106 | 氰戊菊酯 | 0.010 | 0.01 | |
53 | 甲拌磷亚砜 | 0.003 | 0.01 | 107 | 溴氰菊酯 | 0.010 | 0.01 | |
54 | 噻唑滕 | 0.003 | 0.01 |
结论
本文依据GB 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》,采用禾信GC-TQ 6000对黄瓜进行加标回收实验,结果显示107种农药化合物的线性相关系数R均大于0.995;黄瓜基质加标精密度在1.00%-14.54%范围,加标回收率在65.8%-121.2%范围;方法定量限范围为0.001 mg/kg-0.010 mg/kg。上述结果表明禾信GC-TQ 6000具有优异的重现性和检测灵敏度,满足检测需求。
参考文献
1. GB 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》
附录
表3. 107种农药和内标的保留时间和特征离子信息表
序号 | 名 称 | CAS | RT,min | 定量离子对 | 碰撞能V | 定性离子对 | 碰撞能V | |
1 | 敌敌畏 | 62-73-7 | 8.858 | 109.0->79.0 | 5 | 185.0->93.0 | 10 | |
2 | 甲胺磷 | 10265-92-6 | 10.635 | 141.0->95.0 | 5 | 141.0->79.0 | 10 | |
3 | 敌草腈 | 1194-65-6 | 11.228 | 171.0->100.0 | 20 | 171.0->136.0 | 10 | |
4 | 速灭磷1 | 7786-34-7 | 13.057 | 127.0->109.0 | 5 | 127.0->95.0 | 10 | |
5 | 速灭磷2 | 7786-34-7 | 13.268 | 127.0->109.0 | 5 | 127.0->95.0 | 10 | |
6 | 虫螨畏 | 62610-77-9 | 13.800 | 207.9->180.0 | 5 | 207.9->93.0 | 10 | |
7 | 禾草敌 | 2212-67-1 | 13.814 | 126.2->55.1 | 10 | 126.2->83.1 | 5 | |
8 | 环草敌 | 1134-23-2 | 15.421 | 154.1->83.1 | 5 | 154.1->72.1 | 5 | |
9 | 异丙威 | 2631-40-5 | 15.589 | 121.0->77.1 | 10 | 136.0->121.0 | 5 | |
10 | 乙酰甲胺磷 | 30560-19-1 | 15.736 | 136.0->94.0 | 10 | 136.0->42.0 | 5 | |
11 | 六氯苯 | 118-74-1 | 15.981 | 283.8->248.8 | 10 | 283.8->213.9 | 25 | |
12 | 灭线磷 | 13194-48-4 | 16.486 | 157.9->97.0 | 10 | 157.9->114.0 | 5 | |
13 | 乙丁烯氟灵 | 55283-68-6 | 16.878 | 275.9->202.1 | 10 | 315.9->275.9 | 5 | |
14 | 残杀威 | 114-26-1 | 17.473 | 110.0->64.0 | 10 | 110.0->63.0 | 20 | |
15 | 治螟磷 | 3689-24-5 | 17.634 | 237.8->145.9 | 10 | 201.8->145.9 | 5 | |
16 | α-六六六 | 319-84-6 | 18.174 | 218.9->183.0 | 5 | 216.9->181.0 | 5 | |
17 | 脱乙基莠去津 | 6190-65-4 | 19.077 | 187.0->172.0 | 5 | 172.0->94.0 | 10 | |
18 | 特丁硫磷 | 13071-79-9 | 19.093 | 230.9->129.0 | 20 | 230.9->175.0 | 10 | |
19 | 敌噁磷 | 78-34-2 | 19.093 | 125.0->97.0 | 5 | 153.0->97.0 | 5 | |
20 | 野麦畏 | 2303-17-5 | 19.264 | 268.0->184.1 | 10 | 142.9->83.0 | 10 | |
21 | 环丙氟灵 | 26399-36-0 | 19.413 | 317.9->199.0 | 10 | 317.9->54.8 | 10 | |
22 | 地虫硫磷 | 944-22-9 | 19.545 | 136.9->109.0 | 5 | 245.9->137.0 | 5 | |
23 | 丁基嘧啶磷 | 96182-53-5 | 19.662 | 260.8->137.2 | 10 | 233.9->110.1 | 10 | |
24 | 扑灭津 | 139-40-2 | 20.044 | 214.2->172.2 | 5 | 229.1->58.1 | 10 | |
25 | 氯硝胺 | 99-30-9 | 20.271 | 206.1->176.0 | 5 | 160.1->124.1 | 5 | |
26 | 胺丙畏 | 31218-83-4 | 20.388 | 138.0->110.0 | 5 | 138.0->64.0 | 10 | |
27 | 异稻瘟净 | 26087-47-8 | 20.874 | 203.9->91.0 | 5 | 121.9->121.0 | 10 | |
28 | 除线磷 | 97-17-6 | 20.992 | 278.9->222.9 | 10 | 222.9->204.9 | 10 | |
29 | 抗蚜威 | 23103-98-2 | 21.056 | 238.0->166.2 | 10 | 166.0->55.1 | 10 | |
30 | 久效磷 | 6923-22-4 | 21.316 | 127.1->109.0 | 10 | 127.1->95.0 | 10 | |
31 | 乐果 | 60-51-5 | 21.617 | 86.9->46.0 | 10 | 142.9->111.0 | 5 | |
32 | 乙草胺 | 34256-82-1 | 21.917 | 222.9->132.2 | 10 | 222.9->147.2 | 5 | |
33 | 甲草胺 | 15972-60-8 | 22.304 | 188.1->160.2 | 5 | 160.2->132.1 | 5 | |
34 | 甲基嘧啶磷 | 29232-93-7 | 22.486 | 290.0->125.0 | 15 | 232.9->151.0 | 5 | |
35 | 甲基对氧磷 | 950-35-6 | 22.652 | 229.9->136.0 | 5 | 229.9->106.0 | 10 | |
36 | 乙烯菌核利 | 50471-44-8 | 22.762 | 197.9->145.0 | 10 | 187.0->124.0 | 10 | |
37 | 嗪草酮 | 21087-64-9 | 22.92 | 198.0->82.0 | 10 | 198.0->55.0 | 25 | |
38 | 甲霜灵 | 57837-19-1 | 23.015 | 234.0->146.1 | 10 | 220.0->192.1 | 5 | |
39 | 禾草丹 | 28249-77-6 | 23.173 | 100.0->72.0 | 5 | 124.9->89.0 | 10 | |
40 | 异丙甲草胺 | 51218-45-2 | 23.684 | 238.0->162.2 | 10 | 162.2->133.2 | 10 | |
41 | 安硫磷 | 2540-82-1 | 23.771 | 170.0->93.0 | 10 | 197.9->92.9 | 5 | |
42 | 三氯杀螨醇 | 115-32-2 | 23.899 | 139.0->111.0 | 10 | 250.9->138.9 | 10 | |
43 | 倍硫磷 | 55-38-9 | 23.986 | 278.0->109.0 | 10 | 278.0->169.0 | 10 | |
44 | 溴硫磷 | 2104-96-3 | 24.04 | 330.8->315.8 | 10 | 328.8->313.8 | 10 | |
45 | 对氧磷 | 311-45-5 | 24.328 | 108.9->91.0 | 5 | 148.9->119.0 | 5 | |
46 | 环氧七氯B (内标) | 1024-57-3 | 24.415 | 352.8->262.9 | 15 | 354.8->264.9 | 15 | |
47 | 三唑酮 | 43121-43-3 | 24.844 | 208.0->181.1 | 5 | 208.0->111.0 | 10 | |
48 | 烯丙菊酯 | 584-79-2 | 24.851 | 123.0->81.0 | 5 | 107.0->91.0 | 5 | |
49 | 对硫磷 | 56-38-2 | 25.005 | 290.9->109.0 | 10 | 138.9->109.0 | 5 | |
50 | 甲基异柳磷 | 99675-03-3 | 25.072 | 199.0->121.0 | 10 | 241.1->199.1 | 5 | |
51 | 异柳磷 | 25311-71-1 | 25.404 | 212.9->121.1 | 10 | 212.9->185.1 | 5 | |
52 | α-硫丹 | 959-98-8 | 25.436 | 194.9->159.0 | 5 | 194.9->125.0 | 20 | |
53 | 喹硫磷 | 13593-03-8 | 25.56 | 146.0->118.0 | 10 | 146.0->91.0 | 30 | |
54 | 戊菌唑 | 66246-88-6 | 25.835 | 248.0->157.0 | 25 | 248.0->192.0 | 10 | |
55 | 甲拌磷亚砜 | 2588-03-6 | 26.134 | 199.0->142.9 | 5 | 96.9->64.9 | 20 | |
56 | 噻唑滕1 | 98886-44-3 | 26.296 | 195.0->103.0 | 5 | 195.0->60.0 | 20 | |
57 | 4,4'-滴滴伊 | 72-55-9 | 26.327 | 246.1->176.2 | 25 | 315.8->246.0 | 10 | |
58 | 噻唑滕2 | 98886-44-3 | 26.396 | 195.0->103.0 | 5 | 195.0->60.0 | 20 | |
59 | 苯硫威 | 62850-32-2 | 26.477 | 160.1->72.0 | 10 | 72.0->56.0 | 15 | |
60 | 嘧菌胺 | 110235-47-7 | 26.706 | 223.2->222.2 | 10 | 222.2->207.2 | 10 | |
61 | 脱叶磷 | 78-48-8 | 26.753 | 202.0->147.0 | 10 | 169.0->57.1 | 10 | |
62 | 甲拌磷砜 | 2588-04-7 | 26.912 | 153.0->97.0 | 5 | 124.9->96.9 | 5 | |
63 | 除草定 | 314-40-9 | 26.99 | 205.0->188.0 | 10 | 207.0->190.0 | 10 | |
64 | 三唑醇 | 55219-65-3 | 27.093 | 168.0->70.0 | 5 | 128.0->65.0 | 10 | |
65 | 溴苯烯磷 | 33399-00-7 | 27.093 | 266.9->159.1 | 10 | 268.9->161.1 | 10 | |
66 | 丙草胺 | 51218-49-6 | 27.251 | 162.0->132.0 | 10 | 262.0->202.0 | 5 | |
67 | 2,4'-滴滴滴 | 53-19-0 | 27.402 | 235.0->165.2 | 20 | 237.0->165.2 | 20 | |
68 | 醚菌酯 | 143390-89-0 | 27.465 | 116.0->89.0 | 5 | 116.0->63.0 | 30 | |
69 | 异狄氏剂 | 72-20-8 | 27.536 | 262.8->193.0 | 25 | 244.8->173.0 | 20 | |
70 | 灭菌磷 | 5131-24-8 | 27.536 | 130.0->102.1 | 10 | 148.0->130.1 | 15 | |
71 | 噁草酮 | 19666-30-9 | 27.567 | 174.9->112.0 | 15 | 174.9->76.0 | 35 | |
72 | 2,4-滴滴涕 | 789-02-6 | 27.888 | 235.0->165.0 | 20 | 237.0->165.0 | 20 | |
73 | 抑霉唑 | 35554-44-0 | 27.916 | 214.9->173.0 | 5 | 216.8->175.0 | 5 | |
74 | 地胺磷 | 950-10-7 | 28.137 | 168.0->139.9 | 5 | 196.0->139.9 | 10 | |
75 | 环氟菌胺 | 180409-60-3 | 28.156 | 118.1->90.0 | 5 | 118.1->89.0 | 10 | |
76 | 虫螨磷1 | 60238-56-4 | 28.292 | 324.8->268.9 | 10 | 296.8->268.9 | 5 | |
77 | 乙嘧酚磺酸酯 | 41483-43-6 | 28.382 | 272.9->193.1 | 5 | 272.9->108.0 | 10 | |
78 | 乙氧氟草醚 | 42874-03-3 | 28.687 | 252.0->146.0 | 25 | 252.0->196.0 | 15 | |
79 | 虫螨磷2 | 60238-56-4 | 28.741 | 324.8->268.9 | 10 | 296.8->268.9 | 5 | |
80 | 噁唑啉 | 18854-01-8 | 28.754 | 177.1->130.0 | 5 | 177.1->116.0 | 10 | |
81 | 氟酰胺 | 66332-96-5 | 28.828 | 173.0->145.1 | 10 | 280.9->173.0 | 10 | |
82 | 4,4'-滴滴滴 | 72-54-8 | 28.922 | 234.9->165.1 | 20 | 236.9->165.2 | 20 | |
83 | β-硫丹 | 33213-65-9 | 29.029 | 206.9->172.0 | 10 | 194.9->124.9 | 20 | |
84 | 喹氧灵 | 124495-18-7 | 29.19 | 237.0->208.1 | 20 | 271.9->237.1 | 10 | |
85 | 苯草醚 | 74070-46-5 | 29.357 | 264.1->194.2 | 10 | 212.1->182.2 | 10 | |
86 | 肟菌酯 | 141517-21-7 | 29.371 | 116.0->89.0 | 10 | 131.0->89.0 | 20 | |
87 | 三硫磷 | 786-19-6 | 29.438 | 153.0->96.9 | 5 | 199.0->143.0 | 5 | |
88 | 增效醚 | 51-03-6 | 29.585 | 176.0->103.0 | 20 | 176.0->131.0 | 15 | |
89 | 敌瘟磷 | 17109-49-8 | 29.93 | 172.9->109.0 | 10 | 201.0->109.0 | 10 | |
90 | 丰索磷 | 115-90-2 | 30.103 | 291.8->156.0 | 10 | 291.8->108.8 | 10 | |
91 | 联苯菊酯 | 82657-04-3 | 30.197 | 181.2->165.2 | 20 | 181.2->166.2 | 10 | |
92 | 三唑磷 | 24017-47-8 | 30.217 | 161.2->134.2 | 5 | 161.2->106.1 | 10 | |
93 | 吡螨胺 | 119168-77-3 | 30.689 | 275.9->171.1 | 10 | 332.9->171.0 | 15 | |
94 | 溴螨酯 | 18181-80-1 | 30.904 | 185.0->157.0 | 10 | 183.0->155.0 | 10 | |
95 | 胺菊酯1 | 7696-12-0 | 30.911 | 164.0->107.0 | 10 | 164.0->77.0 | 20 | |
96 | 氟环唑 | 133855-98-8 | 30.974 | 192.0->138.0 | 5 | 192.0->111.0 | 15 | |
97 | 胺菊酯2 | 7696-12-0 | 31.079 | 164.0->107.0 | 10 | 164.0->77.0 | 20 | |
98 | 戊唑醇 | 107534-96-3 | 31.142 | 250.0->125.0 | 10 | 250.0->153.0 | 5 | |
99 | 吡丙醚 | 95737-68-1 | 31.339 | 136.0->78.0 | 10 | 136.0->96.0 | 10 | |
100 | 哌草磷 | 24151-93-7 | 31.479 | 320.0->122.0 | 10 | 140.0->98.0 | 5 | |
101 | 苯硫磷 | 2104-64-5 | 31.556 | 169.0->141.1 | 5 | 169.0->77.1 | 10 | |
102 | 环嗪酮 | 51235-04-2 | 31.605 | 171.0->71.1 | 5 | 171.0->85.1 | 10 | |
103 | 咪唑菌酮 | 161326-34-7 | 31.633 | 238.0->237.2 | 5 | 268.0->180.2 | 20 | |
104 | 三氯杀螨砜 | 116-29-0 | 31.931 | 158.9->131.0 | 5 | 226.9->199.0 | 10 | |
105 | 莎稗磷 | 64249-01-0 | 32.043 | 225.9->184.0 | 10 | 255.9->157.0 | 5 | |
106 | 氯菊酯1 | 52645-53-1 | 32.424 | 183.1->168.1 | 10 | 183.1->153.0 | 10 | |
107 | 氯菊酯2 | 52645-53-1 | 32.659 | 183.1->168.1 | 10 | 183.1->153.0 | 10 | |
108 | 氯苯嘧啶醇 | 60168-88-9 | 32.702 | 251.0->139.1 | 10 | 219.0->107.0 | 10 | |
109 | 哒螨灵 | 96489-71-3 | 33.026 | 147.2->132.2 | 10 | 147.2->117.1 | 20 | |
110 | 氯氰菊酯1 | 52315-07-8 | 34.393 | 163.0->91.0 | 10 | 163.0->109.0 | 10 | |
111 | 氯氰菊酯2 | 52315-07-8 | 34.659 | 163.0->91.0 | 10 | 163.0->109.0 | 10 | |
112 | 氯氰菊酯3 | 52315-07-8 | 34.729 | 163.0->91.0 | 10 | 163.0->109.0 | 10 | |
113 | 氯氰菊酯4 | 52315-07-8 | 34.877 | 163.0->91.0 | 10 | 163.0->109.0 | 10 | |
114 | 啶酰菌胺 | 188425-85-6 | 35.391 | 140.0->112.0 | 5 | 140.0->76.0 | 15 | |
115 | 氰戊菊酯1 | 51630-58-1 | 36.018 | 167.0->125.0 | 10 | 224.9->119.0 | 10 | |
116 | 氰戊菊酯2 | 51630-58-1 | 36.484 | 167.0->125.0 | 10 | 224.9->119.0 | 10 | |
117 | 溴氰菊酯 | 52918-63-5 | 37.812 | 250.7->172.0 | 5 | 252.9->93.0 | 10 |
表4.107种农药化合物黄瓜基质加标精密度
序号 | 化合物 | 加标量(mg/kg) | 序号 | 化合物 | 加标量(mg/kg) | 0.01 | 0.05 | 0.1 | 0.01 | 0.05 | 0.1 | ||||||
1 | 敌敌畏 | 70.6% | 74.6% | 72.47% | 55 | 4,4'-滴滴伊 | 100.3% | 101.6% | 98.0% | ||||||||
2 | 甲胺磷 | 72.3% | 80.7% | 83.43% | 56 | 苯硫威 | 87.8% | 97.7% | 99.2% | ||||||||
3 | 敌草腈 | 73.2% | 68.6% | 70.3% | 57 | 嘧菌胺 | 85.5% | 87.0% | 84.8% | ||||||||
4 | 速灭磷 | 77.4% | 91.4% | 92.3% | 58 | 脱叶磷 | 81.7% | 89.0% | 88.6% | ||||||||
5 | 虫螨畏 | 78.7% | 85.6% | 79.0% | 59 | 甲拌磷砜 | 82.9% | 92.8% | 97.9% | ||||||||
6 | 禾草敌 | 71.3% | 81.2% | 80.6% | 60 | 除草定 | 79.0% | 101.6% | 104.6% | ||||||||
7 | 环草敌 | 75.9% | 90.7% | 86.6% | 61 | 三唑醇 | 86.5% | 97.6% | 99.9% | ||||||||
8 | 异丙威 | 84.8% | 90.5% | 91.2% | 62 | 溴苯烯磷 | 81.1% | 100.4% | 92.9% | ||||||||
9 | 乙酰甲胺磷 | 76.0% | 78.6% | 83.5% | 63 | 丙草胺 | 86.2% | 94.7% | 99.6% | ||||||||
10 | 六氯苯 | 83.5% | 77.6% | 82.1% | 64 | 2,4'-滴滴滴 | 95.7% | 108.9% | 101.6% | ||||||||
11 | 灭线磷 | 78.2% | 92.2% | 91.0% | 65 | 醚菌酯 | 95.4% | 103.8% | 100.4% | ||||||||
12 | 乙丁烯氟灵 | 72.0% | 89.2% | 88.7% | 66 | 异狄氏剂 | 93.7% | 99.9% | 98.1% | ||||||||
13 | 残杀威 | 84.5% | 97.7% | 93.4% | 67 | 灭菌磷 | 65.8% | 66.0% | 68.1% | ||||||||
14 | 治螟磷 | 75.9% | 95.2% | 89.3% | 68 | 噁草酮 | 91.8% | 98.2% | 98.0% | ||||||||
15 | α-六六六 | 75.6% | 90.2% | 85.7% | 69 | 2,4-滴滴涕 | 75.1% | 85.6% | 89.2% | ||||||||
16 | 脱乙基莠去津 | 88.0% | 94.3% | 96.8% | 70 | 抑霉唑 | 84.7% | 95.7% | 94.2% | ||||||||
17 | 特丁硫磷 | 75.4% | 98.2% | 88.6% | 71 | 地胺磷 | 89.4% | 94.0% | 95.7% | ||||||||
18 | 敌噁磷 | 82.2% | 97.2% | 90.9% | 72 | 环氟菌胺 | 99.4% | 107.7% | 105.2% | ||||||||
19 | 野麦畏 | 89.5% | 97.0% | 92.1% | 73 | 虫螨磷 | 88.6% | 87.7% | 97.6% | ||||||||
20 | 环丙氟灵 | 83.8% | 85.1% | 95.4% | 74 | 乙嘧酚磺酸酯 | 86.9% | 91.0% | 97.1% | ||||||||
21 | 地虫硫磷 | 89.1% | 92.5% | 93.5% | 75 | 乙氧氟草醚 | 90.4% | 104.3% | 104.5% | ||||||||
22 | 丁基嘧啶磷 | 82.6% | 95.4% | 92.2% | 76 | 噁唑啉 | 94.8% | 88.1% | 94.1% | ||||||||
23 | 扑灭津 | 88.2% | 102.4% | 94.1% | 77 | 氟酰胺 | 115.6% | 101.1% | 108.5% | ||||||||
24 | 氯硝胺 | 93.6% | 96.8% | 100.5% | 78 | 4,4'-滴滴滴 | 95.2% | 108.1% | 103.8% | ||||||||
25 | 胺丙畏 | 82.3% | 89.7% | 99.4% | 79 | β-硫丹 | 95.6% | 99.8% | 101.1% | ||||||||
26 | 异稻瘟净 | 95.4% | 90.9% | 86.4% | 80 | 喹氧灵 | 84.5% | 92.4% | 94.8% | ||||||||
27 | 除线磷 | 83.8% | 93.2% | 92.6% | 81 | 苯草醚 | 99.2% | 103.5% | 102.6% | ||||||||
28 | 抗蚜威 | 87.0% | 91.8% | 92.7% | 82 | 肟菌酯 | 83.9% | 98.4% | 101.2% | ||||||||
29 | 久效磷 | 85.1% | 102.4% | 98.3% | 83 | 三硫磷 | 90.1% | 95.1% | 101.1% | ||||||||
30 | 乐果 | 98.8% | 110.9% | 103.1% | 84 | 增效醚 | 92.0% | 100.2% | 102.4% | ||||||||
31 | 乙草胺 | 88.7% | 103.3% | 92.8% | 85 | 敌瘟磷 | 85.7% | 94.8% | 96.3% | ||||||||
32 | 甲草胺 | 87.9% | 92.3% | 94.0% | 86 | 丰索磷 | 121.2% | 115.6% | 109.5% | ||||||||
33 | 甲基嘧啶磷 | 87.7% | 96.2% | 92.8% | 87 | 联苯菊酯 | 116.8% | 109.8% | 108.7% | ||||||||
34 | 甲基对氧磷 | 87.0% | 97.0% | 100.6% | 88 | 三唑磷 | 92.6% | 99.4% | 96.3% | ||||||||
35 | 乙烯菌核利 | 87.4% | 97.4% | 94.5% | 89 | 吡螨胺 | 87.5% | 98.3% | 95.7% | ||||||||
36 | 嗪草酮 | 86.5% | 99.4% | 95.3% | 90 | 溴螨酯 | 94.7% | 103.7% | 100.9% | ||||||||
37 | 甲霜灵 | 112.9% | 117.8% | 113.3% | 91 | 胺菊酯 | 101.7% | 107.9% | 102.6% | ||||||||
38 | 禾草丹 | 89.6% | 106.0% | 93.4% | 92 | 氟环唑 | 91.5% | 101.2% | 100.7% | ||||||||
39 | 异丙甲草胺 | 95.4% | 99.2% | 95.1% | 93 | 戊唑醇 | 90.1% | 103.6% | 99.3% | ||||||||
40 | 安硫磷 | 68.6% | 66.38% | 67.2% | 94 | 吡丙醚 | 93.0% | 94.3% | 104.6% | ||||||||
41 | 三氯杀螨醇 | 98.1% | 111.5% | 113.0% | 95 | 哌草磷 | 90.5% | 95.9% | 100.7% | ||||||||
42 | 倍硫磷 | 83.8% | 91.0% | 94.1% | 96 | 苯硫磷 | 95.6% | 104.7% | 105.0% | ||||||||
43 | 溴硫磷 | 81.8% | 81.4% | 90.6% | 97 | 环嗪酮 | 92.9% | 98.9% | 98.7% | ||||||||
44 | 对氧磷 | 103.9% | 112.1% | 108.0% | 98 | 咪唑菌酮 | 96.9% | 106.7% | 102.5% | ||||||||
45 | 三唑酮 | 88.7% | 98.4% | 95.4% | 99 | 三氯杀螨砜 | 92.9% | 97.3% | 104.3% | ||||||||
46 | 烯丙菊酯 | 77.3% | 79.7% | 70.5% | 100 | 莎稗磷 | 86.9% | 97.0% | 93.6% | ||||||||
47 | 对硫磷 | 82.5% | 98.9% | 90.4% | 101 | 氯菊酯 | 99.0% | 104.8% | 99.6% | ||||||||
48 | 甲基异柳磷 | 84.7% | 94.7% | 95.6% | 102 | 氯苯嘧啶醇 | 90.9% | 105.1% | 95.7% | ||||||||
49 | 异柳磷 | 86.2% | 91.0% | 88.4% | 103 | 哒螨灵 | 101.4% | 94.9% | 90.9% | ||||||||
50 | α-硫丹 | 108.4% | 101.1% | 99.9% | 104 | 氯氰菊酯 | 90.6% | 97.6% | 96.3% | ||||||||
51 | 喹硫磷 | 82.4% | 88.6% | 96.3% | 105 | 啶酰菌胺 | 88.65% | 92.0% | 100.1% | ||||||||
52 | 戊菌唑 | 86.3% | 100.5% | 96.4% | 106 | 氰戊菊酯 | 91.6% | 100.2% | 99.5% | ||||||||
53 | 甲拌磷亚砜 | 85.7% | 95.2% | 96.0% | 107 | 溴氰菊酯 | 77.7% | 76.9% | 82.6% | ||||||||
54 | 噻唑滕 | 88.3% | 96.8% | 95.5% |
GB 23200.113-2018 B组分析果蔬中113种农药
前言
农药是农业上用于防治病虫害及调节植物生长的化学试剂,广泛用于农林牧业生产、环境和家庭卫生除害防疫、工业品防霉和防蛀等。农药的大量使用容易会导致其在食物链及环境中残留,对人类健康和生态环境造成潜在的危害。因此,建立各类果蔬中农药残留的准确定性定量方法,为老百姓食品安全提供重要保障。
本文参考《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》标准(GB 23200.113-2018),使用气相色谱-串联三重四极杆质谱联用仪对黄瓜基质中的113多种农药及相关化学品进行检测分析,通过定量限、精密度和准确度等指标评估仪器性能,证明GC-TQ 6000满足检测的需要。
实验部分
样品前处理
准确称取10 g黄瓜样品于50 mL离心管中,加入10 mL乙腈和1包QuEChERS萃取盐包,盖上离心管,剧烈振荡3 min后4200 r/min离心5 min。吸取6 mL上清液加到内含净化盐包的15 mL离心管中,涡旋混匀2 min。4200 r/min离心5 min,准确吸取2 mL上清液于10 mL试管中,40℃水浴氮吹近干。加入10 μL内标溶液,1mL乙酸乙酯溶液复溶,过0.22 μm有机滤膜,待测。
仪器条件
表1. 仪器方法参数
模块 | 参数 | 值 |
色谱 | 进样口温度 | 280 °C |
进样方式 | 不分流 | |
色谱柱 | VF-1701MS, 30 m × 0.25 mm × 0.25 μm | |
升温程序 | 起始温度40°C,保持1 min,以40°C/min升至120 °C,再以5 °C/min升至240 °C,再以12℃/min升至300℃,保持6min | |
载气 | 氦气 | |
柱流量 | 1.0 mL/min 恒流模式 | |
质谱 | 离子源 | EI,70eV |
离子源温度 | 280 °C | |
传输线温度 | 280 °C | |
检测器电压 | -1300 V | |
溶剂延迟 碰撞气流量 射出电压(CXP) | 4min 20psi 3V | |
采集模式 | MRM |
结果与讨论
1、标准谱图和物质信息
实验总离子流图见图1,113种农药目标化合物浓度为500 μg/L,内标物浓度为100 μg/L。113种目标化合物以及内标的保留时间以及特征离子信息见附录表3。
图1 113种农药目标化合物总离子流图(500 μg/L)
2、标准曲线
黄瓜空白基质溶液氮吹近干,分别加入1 mL浓度为5 μg/L、10 μg/L、20 μg/L、50 μg/L、100 μg/L、200 μg/L、500 μg/L,内标含量为100 μg/L的混合标准曲线溶液进行分析。113种农药的线性相关系数R均大于0.995。
(a)硫草敌 (b)水胺硫磷 (c)蝇毒磷
图2 三种代表性农药目标化合物的标准曲线图
3、黄瓜加标回收实验
3.1 精密度和准确度
分别对10g黄瓜样品进行加标浓度为0.01 mg/kg、0.05 mg/kg、0.1 mg/kg各六次平行实验,对精密度和准确度进行评估,准确度具体信息详见下附录表4。浓度为0.01 mg/kg、0.05 mg/kg和0.1 mg/kg时,113种农药化合物的相对标准偏差(RSD)分别为4.02%-15.54%、1.14%-9.29%和1.26%-7.66%,回收率分别为70.6%-119.8%、82.1%-119.7%、74.4%-119.3%。
3.2 定量限
按照标准GB/T 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》对10g黄瓜进行加标量为0.01 mg/kg的7次平行回收实验,计算其标准偏差(SD),根据方法定量限LOQ=10×SD计算目标化合物的方法定量限,通过计算可知113种农药化合物的方法定量限为0.003 mg/kg-0.010 mg/kg。
表2.113种农药化合物黄瓜基质加标方法定量限
序号 | 化合物 | 方法 定量限(mg/kg) | 标准要求 方法定量限(mg/kg) | 序号 | 化合物 | 方法 定量限(mg/kg) | 标准要求 方法定量限(mg/kg) | |
1 | 硫草敌 | 0.006 | 0.01 | 58 | 水胺硫磷 | 0.006 | 0.01 | |
2 | 联苯 | 0.007 | 0.01 | 59 | 氯丹-反式 | 0.007 | 0.01 | |
3 | 土菌灵 | 0.006 | 0.01 | 60 | 四氟醚唑 | 0.008 | 0.01 | |
4 | 氯苯甲醚 | 0.007 | 0.01 | 61 | 丁草胺 | 0.007 | 0.01 | |
5 | 四氯硝基苯 | 0.004 | 0.01 | 62 | 丙硫磷 | 0.005 | 0.01 | |
6 | 虫线磷 | 0.005 | 0.01 | 63 | 氟丁酰草胺 | 0.006 | 0.01 | |
7 | 二苯胺 | 0.005 | 0.01 | 64 | 杀虫畏 | 0.006 | 0.01 | |
8 | 仲丁威 | 0.007 | 0.01 | 65 | 腐霉利 | 0.007 | 0.01 | |
9 | 乙丁氟灵 | 0.006 | 0.01 | 66 | 狄氏剂 | 0.003 | 0.01 | |
10 | 二溴磷 | 0.008 | 0.01 | 67 | 杀扑磷 | 0.005 | 0.01 | |
11 | 甲拌磷 | 0.009 | 0.01 | 68 | 丙溴磷 | 0.007 | 0.01 | |
12 | 氯苯胺灵 | 0.010 | 0.01 | 69 | 敌草胺 | 0.006 | 0.01 | |
13 | 五氯硝基苯 | 0.010 | 0.01 | 70 | 己唑醇 | 0.009 | 0.01 | |
14 | 氧乐果 | 0.005 | 0.01 | 71 | 抑草磷 | 0.003 | 0.01 | |
15 | 阿特拉通 | 0.007 | 0.01 | 72 | 多效唑 | 0.006 | 0.01 | |
16 | 二嗪磷 | 0.008 | 0.01 | 73 | 杀螨酯 | 0.008 | 0.01 | |
17 | 异噁草酮 | 0.006 | 0.01 | 74 | 吡氟禾草灵 | 0.007 | 0.01 | |
18 | 百治磷 | 0.006 | 0.01 | 75 | 稻瘟灵 | 0.007 | 0.01 | |
19 | 嘧霉胺 | 0.006 | 0.01 | 76 | 硫环磷 | 0.006 | 0.01 | |
20 | γ-六六六 | 0.008 | 0.01 | 77 | 乙酯杀螨醇 | 0.006 | 0.01 | |
21 | 乙嘧硫磷 | 0.005 | 0.01 | 78 | 除草醚 | 0.008 | 0.01 | |
22 | 克百威 | 0.006 | 0.01 | 79 | 乙硫磷 | 0.006 | 0.01 | |
23 | 莠去津 | 0.007 | 0.01 | 80 | 三氟硝草醚 | 0.008 | 0.01 | |
24 | 西玛津 | 0.010 | 0.01 | 81 | 4,4'-滴滴涕 | 0.007 | 0.01 | |
25 | 特丁津 | 0.007 | 0.01 | 82 | 烯唑醇 | 0.005 | 0.01 | |
26 | 绿谷隆 | 0.006 | 0.01 | 83 | 腈菌唑 | 0.005 | 0.01 | |
27 | 五氯苯胺 | 0.006 | 0.01 | 84 | 环丙唑醇 | 0.007 | 0.01 | |
28 | 氯唑磷 | 0.005 | 0.01 | 85 | 苯霜灵 | 0.007 | 0.01 | |
29 | 炔苯酰草胺 | 0.005 | 0.01 | 86 | 氟虫腈 | 0.006 | 0.01 | |
30 | 甲基毒死蜱 | 0.004 | 0.01 | 87 | 丙环唑 | 0.008 | 0.01 | |
31 | 艾氏剂 | 0.007 | 0.01 | 88 | 禾草灵 | 0.007 | 0.01 | |
32 | 皮蝇磷 | 0.006 | 0.01 | 89 | 倍硫磷亚砜 | 0.010 | 0.01 | |
33 | 敌草净 | 0.006 | 0.01 | 90 | 倍硫磷砜 | 0.010 | 0.01 | |
34 | 甲基立枯磷 | 0.005 | 0.01 | 91 | 咯菌腈 | 0.008 | 0.01 | |
35 | 扑草净 | 0.004 | 0.01 | 92 | 噁霜灵 | 0.007 | 0.01 | |
36 | 莠灭净 | 0.007 | 0.01 | 93 | 乙螨唑 | 0.009 | 0.01 | |
37 | β-六六六 | 0.007 | 0.01 | 94 | 异菌脲 | 0.010 | 0.01 | |
38 | 特丁净 | 0.007 | 0.01 | 95 | 甲氧滴滴涕 | 0.007 | 0.01 | |
39 | 毒死蜱 | 0.008 | 0.01 | 96 | 伐灭磷 | 0.008 | 0.01 | |
40 | 磷胺 | 0.006 | 0.01 | 97 | 甲氰菊酯 | 0.007 | 0.01 | |
41 | 马拉氧磷 | 0.006 | 0.01 | 98 | 哒嗪硫磷 | 0.006 | 0.01 | |
42 | 异丙净 | 0.005 | 0.01 | 99 | 溴苯磷 | 0.006 | 0.01 | |
43 | 甲基对硫磷 | 0.006 | 0.01 | 100 | 亚胺硫磷 | 0.003 | 0.01 | |
44 | 毒壤滕 | 0.005 | 0.01 | 101 | 甲羧除草醚 | 0.010 | 0.01 | |
45 | δ-六六六 | 0.006 | 0.01 | 102 | 氯氟氰菊酯 | 0.009 | 0.01 | |
46 | 嘧啶磷 | 0.006 | 0.01 | 103 | 氟丙菊酯 | 0.009 | 0.01 | |
47 | 马拉硫磷 | 0.006 | 0.01 | 104 | 伏杀硫磷 | 0.008 | 0.01 | |
48 | 烯虫酯 | 0.005 | 0.01 | 105 | 苯噻酰草胺 | 0.009 | 0.01 | |
49 | 杀螟硫磷 | 0.005 | 0.01 | 106 | 益棉磷 | 0.010 | 0.01 | |
50 | 乙氧呋草黄 | 0.008 | 0.01 | 107 | 氟喹唑 | 0.006 | 0.01 | |
51 | 嘧菌环胺 | 0.006 | 0.01 | 108 | 氟氯氰菊酯 | 0.010 | 0.01 | |
52 | 氧异柳磷 | 0.005 | 0.01 | 109 | 蝇毒磷 | 0.006 | 0.01 | |
53 | 二甲戊灵 | 0.005 | 0.01 | 110 | 氟氰戊菊酯 | 0.008 | 0.01 | |
54 | 毒虫畏 | 0.003 | 0.01 | 111 | 腈苯唑 | 0.007 | 0.01 | |
55 | 敌稗 | 0.007 | 0.01 | 112 | 氟胺氰菊酯 | 0.009 | 0.01 | |
56 | o,p'-DDE | 0.008 | 0.01 | 113 | 苯醚甲环唑 | 0.006 | 0.01 | |
57 | 乙基溴硫磷 | 0.006 | 0.01 |
结论
本文依据GB 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》,采用禾信GC-TQ 6000对黄瓜进行加标回收实验,结果显示113种农药化合物的线性相关系数R均大于0.995;黄瓜基质加标精密度在1.14%-15.54%范围,加标回收率在70.6%-119.8%范围;方法定量限在0.003 mg/kg-0.010 mg/kg范围内。上述结果表明禾信GC-TQ 6000具有优异的重现性和检测灵敏度,满足检测需求。
参考文献
1. GB 23200.113-2018《食品安全国家标准 植物源性食品中208种农药及其代谢物残留量的测定 气相色谱-质谱联用法》
附录
表3. 113种农药和内标的保留时间和特征离子信息表
序号 | 名 称 | CAS | RT,min | 定量离子对 | 碰撞能V | 定性离子对 | 碰撞能V | |
1 | 硫草敌 | 2941-55-1 | 7.154 | 100.0->72.0 | 5 | 161.0->100.0 | 5 | |
2 | 联苯 | 92-52-4 | 10.299 | 154.0->153.0 | 10 | 153.0->152.0 | 10 | |
3 | 土菌灵 | 2593-15-9 | 11.761 | 211.0->183.0 | 5 | 183.0->140.0 | 10 | |
4 | 氯苯甲醚 | 2675-77-6 | 13.539 | 191.0->113.0 | 10 | 191.0->141.0 | 5 | |
5 | 四氯硝基苯 | 117-18-0 | 15.111 | 260.9->203.0 | 10 | 214.9->179.0 | 5 | |
6 | 虫线磷 | 297-97-2 | 16.186 | 143.0->79.0 | 5 | 175.0->79.0 | 5 | |
7 | 二苯胺 | 122-39-4 | 16.699 | 169.0->168.2 | 10 | 168.0->167.2 | 10 | |
8 | 仲丁威 | 3766-81-2 | 16.96 | 121.0->77.0 | 15 | 121.0->103.1 | 10 | |
9 | 乙丁氟灵 | 1861-40-1 | 17.347 | 292.0->264.0 | 5 | 292.0->206.0 | 5 | |
10 | 二溴磷 | 300-76-5 | 17.506 | 108.9->79.0 | 5 | 144.9->109.0 | 5 | |
11 | 甲拌磷 | 298-02-2 | 17.632 | 260.0->75.0 | 5 | 230.9->128.9 | 15 | |
12 | 氯苯胺灵 | 101-21-3 | 17.924 | 153.0->125.1 | 5 | 153.0->90.0 | 15 | |
13 | 五氯硝基苯 | 82-68-8 | 18.312 | 295.0->237.0 | 10 | 236.9->142.9 | 15 | |
14 | 氧乐果 | 1113-02-6 | 18.972 | 156.0->110.0 | 5 | 110.0->79.0 | 5 | |
15 | 阿特拉通 | 1610-17-9 | 19.081 | 169.0->154.0 | 5 | 211.0->169.0 | 5 | |
16 | 二嗪磷 | 331-41-5 | 19.161 | 137.0->84.0 | 5 | 137.0->54.0 | 15 | |
17 | 异噁草酮 | 81777-89-1 | 19.322 | 125.0->89.0 | 10 | 204.0->107.0 | 15 | |
18 | 百治磷 | 141-66-2 | 19.497 | 127.0->109.0 | 10 | 127.0->95.0 | 10 | |
19 | 嘧霉胺 | 53112-28-0 | 19.607 | 198.0->183.0 | 10 | 198.0->118.0 | 25 | |
20 | γ-六六六 | 58-89-9 | 19.877 | 217.0->181.0 | 5 | 181.0->145.0 | 10 | |
21 | 乙嘧硫磷 | 38260-54-7 | 20.052 | 181.0->153.0 | 5 | 168.0->153.0 | 5 | |
22 | 克百威 | 1563-66-2 | 20.096 | 164.0->149.0 | 5 | 164.0->131.0 | 10 | |
23 | 莠去津 | 1912-24-9 | 20.213 | 215.0->200.0 | 5 | 215.0->58.0 | 10 | |
24 | 西玛津 | 122-34-9 | 20.315 | 201.0->173.0 | 5 | 201.0->186.0 | 5 | |
25 | 特丁津 | 5915-41-3 | 20.483 | 229.0->173.0 | 5 | 173.0->172.0 | 5 | |
26 | 绿谷隆 | 1746-81-2 | 20.774 | 126.0->99.0 | 5 | 214.0->61.0 | 5 | |
27 | 五氯苯胺 | 527-20-8 | 21.028 | 263.0->192.0 | 15 | 265.0->194.0 | 15 | |
28 | 氯唑磷 | 42509-80-8 | 21.02 | 161.0->119.0 | 5 | 161.0->146.0 | 5 | |
29 | 炔苯酰草胺 | 23950-58-5 | 21.204 | 173.0->145.0 | 10 | 175.0->147.0 | 10 | |
30 | 甲基毒死蜱 | 5598-13-0 | 21.502 | 286.0->93.0 | 20 | 288.0->93.0 | 15 | |
31 | 艾氏剂 | 309-00-2 | 21.783 | 263.0->193.0 | 25 | 255.0->220.0 | 10 | |
32 | 皮蝇磷 | 299-84-3 | 22.002 | 285.0->270.0 | 10 | 287.0->272.0 | 10 | |
33 | 敌草净 | 1014-69-3 | 22.072 | 213.0->171.0 | 5 | 213.0->58.0 | 10 | |
34 | 甲基立枯磷 | 57018-04-9 | 22.142 | 265.0->250.0 | 10 | 265.0->93.0 | 20 | |
35 | 扑草净 | 7287-19-6 | 22.528 | 199.0->184.0 | 5 | 226.0->184.0 | 5 | |
36 | 莠灭净 | 834-12-8 | 22.677 | 227.0->170.0 | 5 | 227.0->58.0 | 10 | |
37 | β-六六六 | 319-85-7 | 22.905 | 217.0->181.0 | 5 | 181.0->145.0 | 10 | |
38 | 特丁净 | 886-50-0 | 23.037 | 185.0->170.0 | 5 | 241.0->170.0 | 10 | |
39 | 毒死蜱 | 2921-88-2 | 23.045 | 197.0->169.0 | 10 | 199.0->171.0 | 10 | |
40 | 磷胺-1 | 13171-21-6 | 23.344 | 127.0->109.0 | 5 | 127.0->95.0 | 10 | |
41 | 马拉氧磷 | 1634-72-8 | 23.344 | 127.0->99.0 | 5 | 127.0->55.0 | 5 | |
42 | 异丙净 | 4147-51-7 | 23.405 | 255.0->222.0 | 5 | 255.0->180.0 | 10 | |
43 | 磷胺-2 | 13171-21-6 | 23.528 | 127.0->109.0 | 5 | 127.0->95.0 | 10 | |
44 | 甲基对硫磷 | 298-00-0 | 23.536 | 263.0->109.0 | 5 | 233.0->109.0 | 15 | |
45 | 毒壤滕 | 327-98-0 | 23.387 | 299.0->271.0 | 10 | 297.0->269.0 | 10 | |
46 | δ-六六六 | 319-86-8 | 23.811 | 217.0->181.0 | 5 | 181.0->145.0 | 10 | |
47 | 嘧啶磷 | 23505-41-1 | 23.797 | 318.0->182.0 | 5 | 318.0->166.0 | 5 | |
48 | 马拉硫磷 | 121-75-5 | 24.078 | 127.0->99.0 | 5 | 173.0->99.0 | 10 | |
49 | 烯虫酯 | 40596-69-8 | 24.232 | 153.0->111.0 | 5 | 111.0->55.0 | 10 | |
50 | 杀螟硫磷 | 122-14-5 | 24.288 | 277.0->260.0 | 5 | 277.0->109.0 | 10 | |
51 | 环氧七氯B | 1024-57-3 | 24.449 | 352.8->262.9 | 15 | 354.8->264.9 | 15 | |
52 | 乙氧呋草黄 | 26225-79-6 | 24.575 | 207.0->161.0 | 5 | 161.0->105.0 | 5 | |
53 | 嘧菌环胺 | 121552-61-2 | 24.393 | 225.2->224.3 | 5 | 224.2->208.2 | 15 | |
54 | 氧异柳磷 | 31120-85-1 | 24.825 | 229.0->200.9 | 5 | 229.0->121.0 | 20 | |
55 | 二甲戊灵 | 40487-42-1 | 24.899 | 252.0->162.2 | 5 | 252.0->161.1 | 15 | |
56 | 毒虫畏 | 470-90-6 | 25.609 | 266.9->159.1 | 10 | 322.8->266.8 | 10 | |
57 | 敌稗 | 709-98-8 | 25.569 | 161.0->99.0 | 20 | 161.0->90.0 | 15 | |
58 | o,p'-DDE | 3424-82-6 | 25.073 | 246.0->176.2 | 25 | 248.0->176.2 | 25 | |
59 | 乙基溴硫磷 | 4824-78-6 | 25.348 | 358.7->302.8 | 10 | 302.8->284.7 | 10 | |
60 | 水胺硫磷 | 24353-61-5 | 25.65 | 135.9->108.0 | 10 | 135.9->69.0 | 20 | |
61 | 氯丹-反式 | 5103-74-2 | 25.683 | 372.8->265.8 | 20 | 271.7->236.9 | 10 | |
62 | 四氟醚唑 | 112281-77-3 | 26.219 | 336.0->203.8 | 25 | 336.0->217.9 | 10 | |
63 | 丁草胺 | 23184-66-9 | 26.259 | 236.9->160.2 | 5 | 188.1->160.2 | 5 | |
64 | 丙硫磷 | 34643-46-4 | 26.454 | 267.0->239.0 | 5 | 309.0->239.0 | 10 | |
65 | 氟丁酰草胺 | 113614-08-7 | 27.058 | 176.1->91.1 | 10 | 221.0->193.1 | 5 | |
66 | 杀虫畏 | 22248-79-9 | 26.814 | 329.0->109.0 | 15 | 331.0->109.0 | 10 | |
67 | 腐霉利 | 32809-16-8 | 27.021 | 96.0->67.1 | 5 | 96.0->53.0 | 10 | |
68 | 狄氏剂 | 60-57-1 | 26.856 | 263.0->193.0 | 25 | 277.0->241.0 | 5 | |
69 | 杀扑磷 | 950-37-8 | 27.162 | 144.9->85.0 | 5 | 144.9->58.1 | 10 | |
70 | 丙溴磷 | 41198-08-7 | 27.223 | 338.8->268.7 | 10 | 207.9->63.0 | 25 | |
71 | 敌草胺 | 15299-99-7 | 27.448 | 128.0->72.1 | 5 | 128.0->100.1 | 5 | |
72 | 己唑醇 | 79983-71-4 | 27.577 | 231.0->175.0 | 5 | 256.0->82.1 | 10 | |
73 | 抑草磷 | 36335-67-8 | 27.619 | 286.0->202.0 | 10 | 200.0->92.0 | 5 | |
74 | 多效唑 | 76738-62-0 | 27.986 | 236.0->125.1 | 10 | 236.0->167.0 | 5 | |
75 | 杀螨酯 | 80-33-1 | 27.863 | 175.0->111.0 | 5 | 111.0->75.0 | 10 | |
76 | 吡氟禾草灵 | 69806-50-4 | 28.003 | 281.9->91.0 | 10 | 281.9->238.0 | 10 | |
77 | 稻瘟灵 | 50512-35-1 | 28.135 | 162.1->134.0 | 5 | 162.1->85.0 | 10 | |
78 | 硫环磷 | 947-02-4 | 28.258 | 196.0->140.0 | 5 | 168.0->140.0 | 5 | |
79 | 乙酯杀螨醇 | 510-15-6 | 28.521 | 139.1->111.0 | 10 | 251.1->139.1 | 10 | |
80 | 除草醚 | 1836-75-5 | 28.731 | 202.0->139.1 | 15 | 282.9->253.0 | 5 | |
81 | 乙硫磷 | 563-12-2 | 29.021 | 230.9->129.0 | 15 | 230.9->175.0 | 10 | |
82 | 三氟硝草醚 | 15457-05-3 | 29.336 | 190.0->126.0 | 15 | 190.0->132.0 | 10 | |
83 | 4,4'-滴滴涕 | 50-29-3 | 29.389 | 235.0->165.2 | 15 | 237.0->165.2 | 15 | |
84 | 烯唑醇 | 83657-24-3 | 29.354 | 267.9->232.0 | 5 | 269.9->232.0 | 5 | |
85 | 腈菌唑 | 88671-89-0 | 29.529 | 179.0->125.0 | 10 | 179.0->90.0 | 20 | |
86 | 环丙唑醇-1 | 113096-99-4 | 29.573 | 222.0->125.0 | 10 | 139.1->111.0 | 10 | |
87 | 苯霜灵 | 71626-11-4 | 29.573 | 148.0->77.0 | 25 | 148.0->105.1 | 10 | |
88 | 环丙唑醇-2 | 113096-99-4 | 29.675 | 222.0->125.0 | 10 | 139.1->111.0 | 10 | |
89 | 氟虫腈 | 120068-37-3 | 29.696 | 366.8->212.8 | 20 | 368.8->214.8 | 20 | |
90 | 丙环唑-1 | 60207-90-1 | 29.889 | 172.9->145.0 | 10 | 172.9->74.0 | 25 | |
91 | 丙环唑-2 | 60207-90-1 | 30.011 | 172.9->145.0 | 10 | 172.9->74.0 | 25 | |
92 | 禾草灵 | 51338-27-3 | 29.976 | 339.9->252.9 | 5 | 253.0->162.0 | 10 | |
93 | 倍硫磷亚砜 | 3761-41-9 | 30.24 | 278.0->109.0 | 15 | 278.0->169.0 | 10 | |
94 | 倍硫磷砜 | 3761-42-0 | 30.668 | 309.9->105.0 | 10 | 135.9->92.0 | 5 | |
95 | 咯菌腈 | 131341-86-1 | 30.922 | 248.0->182.0 | 10 | 248.0->154.0 | 15 | |
96 | 噁霜灵 | 77732-09-3 | 30.944 | 163.0->132.0 | 5 | 163.0->117.0 | 20 | |
97 | 乙螨唑 | 153233-91-1 | 30.922 | 141.0->113.0 | 10 | 141.0->63.0 | 20 | |
98 | 异菌脲 | 36734-19-7 | 31.59 | 187.0->124.0 | 10 | 245.0->161.0 | 15 | |
99 | 甲氧滴滴涕 | 72-43-5 | 30.88 | 227.1->169.0 | 15 | 227.1->141.0 | 30 | |
100 | 伐灭磷 | 52-85-7 | 31.156 | 218.0->109.0 | 10 | 218.0->79.0 | 20 | |
101 | 甲氰菊酯 | 39515-41-8 | 31.156 | 207.9->181.0 | 5 | 264.9->210.0 | 5 | |
102 | 哒嗪硫磷 | 119-12-0 | 31.548 | 340.0->199.0 | 5 | 204.0->203.1 | 5 | |
103 | 溴苯磷 | 21609-90-5 | 31.41 | 171.0->77.1 | 15 | 154.9->77.1 | 10 | |
104 | 亚胺硫磷 | 732-11-6 | 31.845 | 160.0->77.1 | 15 | 160.0->133.1 | 5 | |
105 | 甲羧除草醚 | 42576-02-3 | 31.982 | 189.1->126.0 | 15 | 340.9->309.9 | 5 | |
106 | 氯氟氰菊酯-1 | 68085-85-8 | 32.301 | 197.0->141.0 | 10 | 197.0->161.0 | 5 | |
107 | 氟丙菊酯 | 101007-06-1 | 32.301 | 207.9->181.0 | 5 | 288.9->92.8 | 5 | |
108 | 氯氟氰菊酯-2 | 68085-85-8 | 32.396 | 197.0->141.0 | 10 | 197.0->161.0 | 5 | |
109 | 伏杀硫磷 | 2310-17-0 | 32.417 | 182.0->111.0 | 10 | 182.0->102.0 | 10 | |
110 | 苯噻酰草胺 | 73250-68-7 | 32.555 | 192.0->136.1 | 10 | 192.0->109.1 | 20 | |
111 | 益棉磷 | 2642-71-9 | 33.149 | 132.0->77.1 | 10 | 160.0->77.1 | 10 | |
112 | 氟喹唑 | 136426-54-5 | 33.597 | 340.0->298.0 | 10 | 108.0->57.0 | 10 | |
113 | 氟氯氰菊酯-1 | 68359-37-5 | 34.171 | 226.0->206.0 | 10 | 198.9->170.1 | 15 | |
114 | 氟氯氰菊酯-2 | 68359-37-5 | 34.424 | 226.0->206.0 | 10 | 198.9->170.1 | 15 | |
115 | 氟氯氰菊酯-3 | 68359-37-5 | 34.494 | 226.0->206.0 | 10 | 198.9->170.1 | 15 | |
116 | 蝇毒磷 | 56-72-4 | 34.536 | 361.9->109.0 | 10 | 210.0->182.0 | 5 | |
117 | 氟氯氰菊酯-4 | 68359-37-5 | 34.641 | 226.0->206.0 | 10 | 198.9->170.1 | 15 | |
118 | 氟氰戊菊酯-1 | 70124-77-5 | 35.124 | 156.9->107.1 | 10 | 198.9->157.0 | 5 | |
119 | 氟氰戊菊酯-2 | 70124-77-5 | 35.495 | 156.9->107.1 | 10 | 198.9->157.0 | 5 | |
120 | 腈苯唑 | 119611-00-6 | 35.712 | 197.9->129.0 | 5 | 128.9->102.0 | 10 | |
121 | 氟胺氰菊酯-1 | 69409-94-5 | 36.777 | 250.0->200.0 | 10 | 250.0->55.0 | 10 | |
122 | 氟胺氰菊酯-2 | 69409-94-5 | 36.91 | 250.0->200.0 | 10 | 250.0->55.0 | 10 | |
123 | 苯醚甲环唑-1 | 119446-68-3 | 37.464 | 322.8->264.9 | 10 | 264.9->202.0 | 10 | |
124 | 苯醚甲环唑-2 | 119446-68-3 | 37.464 | 322.8->264.9 | 10 | 264.9->202.0 | 10 |
表4.113种农药化合物黄瓜基质加标精密度
序号 | 化合物 | 加标量(mg/kg) | 序号 | 化合物 | 加标量(mg/kg) | 0.01 | 0.05 | 0.1 | 0.01 | 0.05 | 0.1 | ||||||
1 | 硫草敌 | 82.4% | 83.8% | 94.1% | 58 | 水胺硫磷 | 88.3% | 93.3% | 96.0% | ||||||||
2 | 联苯 | 101.0% | 106.8% | 107.2% | 59 | 氯丹-反式 | 86.5% | 87.9% | 92.2% | ||||||||
3 | 土菌灵 | 87.2% | 89.6% | 98.3% | 60 | 四氟醚唑 | 91.7% | 90.4% | 98.4% | ||||||||
4 | 氯苯甲醚 | 94.6% | 94.9% | 96.2% | 61 | 丁草胺 | 89.5% | 94.1% | 99.4% | ||||||||
5 | 四氯硝基苯 | 80.6% | 85.1% | 89.9% | 62 | 丙硫磷 | 86.7% | 90.0% | 94.9% | ||||||||
6 | 虫线磷 | 86.2% | 91.7% | 94.6% | 63 | 氟丁酰草胺 | 91.9% | 93.6% | 99.6% | ||||||||
7 | 二苯胺 | 92.7% | 79.2% | 87.8% | 64 | 杀虫畏 | 89.9% | 92.1% | 98.4% | ||||||||
8 | 仲丁威 | 73.7% | 81.3% | 80.8% | 65 | 腐霉利 | 92.8% | 86.2% | 95.1% | ||||||||
9 | 乙丁氟灵 | 70.6% | 78.4% | 74.4% | 66 | 狄氏剂 | 93.9% | 94.3% | 99.3% | ||||||||
10 | 二溴磷 | 90.4% | 94.2% | 92.0% | 67 | 杀扑磷 | 88.4% | 92.0% | 98.4% | ||||||||
11 | 甲拌磷 | 90.4% | 85.1% | 89.5% | 68 | 丙溴磷 | 85.9% | 84.1% | 84.3% | ||||||||
12 | 氯苯胺灵 | 104.2% | 100.3% | 107.3% | 69 | 敌草胺 | 93.6% | 93.3% | 91.8% | ||||||||
13 | 五氯硝基苯 | 85.8% | 82.1% | 87.8% | 70 | 己唑醇 | 96.1% | 91.3% | 90.1% | ||||||||
14 | 氧乐果 | 82.9% | 88.3% | 84.7% | 71 | 抑草磷 | 76.2% | 82.4% | 81.8% | ||||||||
15 | 阿特拉通 | 87.2% | 91.1% | 87.6% | 72 | 多效唑 | 96.4% | 97.0% | 99.9% | ||||||||
16 | 二嗪磷 | 78.2% | 84.5% | 86.8% | 73 | 杀螨酯 | 107.9% | 108.2% | 106.0% | ||||||||
17 | 异噁草酮 | 74.6% | 81.5% | 83.7% | 74 | 吡氟禾草灵 | 92.4% | 93.6% | 99.4% | ||||||||
18 | 百治磷 | 87.1% | 93.0% | 90.2% | 75 | 稻瘟灵 | 96.7% | 95.5% | 101.9% | ||||||||
19 | 嘧霉胺 | 86.2% | 85.7% | 92.3% | 76 | 硫环磷 | 82.2% | 87.4% | 86.3% | ||||||||
20 | γ-六六六 | 75.3% | 79.9% | 77.2% | 77 | 乙酯杀螨醇 | 105.7% | 100.6% | 105.6% | ||||||||
21 | 乙嘧硫磷 | 78.9% | 83.6% | 83.6% | 78 | 除草醚 | 90.7% | 93.9% | 91.5% | ||||||||
22 | 克百威 | 92.0% | 97.8% | 101.0% | 79 | 乙硫磷 | 99.4% | 101.2% | 104.8% | ||||||||
23 | 莠去津 | 95.5% | 96.0% | 101.4% | 80 | 三氟硝草醚 | 81.0% | 90.5% | 93.8% | ||||||||
24 | 西玛津 | 97.6% | 95.4% | 102.8% | 81 | 4,4'-滴滴涕 | 95.8% | 103.8% | 101.5% | ||||||||
25 | 特丁津 | 95.6% | 95.3% | 99.3% | 82 | 烯唑醇 | 92.1% | 92.3% | 100.9% | ||||||||
26 | 绿谷隆 | 87.4% | 86.4% | 92.5% | 83 | 腈菌唑 | 101.4% | 98.8% | 99.2% | ||||||||
27 | 五氯苯胺 | 78.7% | 82.1% | 88.0% | 84 | 环丙唑醇 | 95.1% | 96.0% | 104.4% | ||||||||
28 | 氯唑磷 | 82.0% | 87.9% | 88.3% | 85 | 苯霜灵 | 104.0% | 97.5% | 107.9% | ||||||||
29 | 炔苯酰草胺 | 93.4% | 95.1% | 101.1% | 86 | 氟虫腈 | 95.1% | 98.6% | 100.9% | ||||||||
30 | 甲基毒死蜱 | 79.9% | 85.2% | 84.6% | 87 | 丙环唑 | 111.9% | 101.0% | 106.7% | ||||||||
31 | 艾氏剂 | 79.8% | 82.6% | 79.8% | 88 | 禾草灵 | 99.9% | 91.3% | 106.9% | ||||||||
32 | 皮蝇磷 | 81.4% | 83.9% | 84.7% | 89 | 倍硫磷亚砜 | 104.7% | 108.1% | 106.1% | ||||||||
33 | 敌草净 | 98.8% | 95.3% | 101.1% | 90 | 倍硫磷砜 | 98.55% | 92.5% | 98.2% | ||||||||
34 | 甲基立枯磷 | 84.7% | 88.3% | 90.2% | 91 | 咯菌腈 | 106.4% | 103.4% | 105.5% | ||||||||
35 | 扑草净 | 94.1% | 93.5% | 101.5% | 92 | 噁霜灵 | 98.7% | 98.4% | 99.4% | ||||||||
36 | 莠灭净 | 94.2% | 93.3% | 100.1% | 93 | 乙螨唑 | 97.0% | 94.7% | 95.5% | ||||||||
37 | β-六六六 | 89.5% | 92.4% | 97.5% | 94 | 异菌脲 | 102.6% | 110.2% | 108.6% | ||||||||
38 | 特丁净 | 93.6% | 92.6% | 99.9% | 95 | 甲氧滴滴涕 | 98.3% | 100.5% | 92.7% | ||||||||
39 | 毒死蜱 | 89.9% | 91.5% | 95.0% | 96 | 伐灭磷 | 101.0% | 100.1% | 107.3% | ||||||||
40 | 磷胺 | 84.2% | 89.5% | 86.8% | 97 | 甲氰菊酯 | 96.7% | 94.3% | 96.2% | ||||||||
41 | 马拉氧磷 | 91.9% | 93.4% | 89.9% | 98 | 哒嗪硫磷 | 95.4% | 89.9% | 95.4% | ||||||||
42 | 异丙净 | 88.5% | 89.2% | 87.2% | 99 | 溴苯磷 | 97.7% | 95.3% | 100.3% | ||||||||
43 | 甲基对硫磷 | 80.0% | 83.6% | 85.1% | 100 | 亚胺硫磷 | 87.4% | 87.1% | 86.2% | ||||||||
44 | 毒壤滕 | 84.4% | 85.9% | 82.5% | 101 | 甲羧除草醚 | 97.65% | 98.8% | 104.1% | ||||||||
45 | δ-六六六 | 94.1% | 92.5% | 90.9% | 102 | 氯氟氰菊酯 | 97.0% | 97.6% | 99.6% | ||||||||
46 | 嘧啶磷 | 83.1% | 86.9% | 92.8% | 103 | 氟丙菊酯 | 92.0% | 92.5% | 95.6% | ||||||||
47 | 马拉硫磷 | 89.1% | 91.8% | 88.2% | 104 | 伏杀硫磷 | 96.1% | 94.2% | 93.7% | ||||||||
48 | 烯虫酯 | 85.7% | 82.7% | 88.1% | 105 | 苯噻酰草胺 | 114.4% | 118.4% | 119.2% | ||||||||
49 | 杀螟硫磷 | 76.4% | 82.3% | 87.0% | 106 | 益棉磷 | 103.5% | 97.5% | 95.5% | ||||||||
50 | 乙氧呋草黄 | 97.8% | 97.2% | 103.1% | 107 | 氟喹唑 | 94.4% | 90.8% | 98.1% | ||||||||
51 | 嘧菌环胺 | 119.8% | 119.7% | 119.3% | 108 | 氟氯氰菊酯 | 100.6% | 106.3% | 104.9% | ||||||||
52 | 氧异柳磷 | 107.7% | 113.1% | 113.4% | 109 | 蝇毒磷 | 96.7% | 93.9% | 103.6% | ||||||||
53 | 二甲戊灵 | 70.6% | 81.5% | 83.9% | 110 | 氟氰戊菊酯 | 101.5% | 101.1% | 107.4% | ||||||||
54 | 毒虫畏 | 87.5% | 91.6% | 87.4% | 111 | 腈苯唑 | 98.1% | 106.7% | 105.7% | ||||||||
55 | 敌稗 | 92.7% | 95.2% | 93.8% | 112 | 氟胺氰菊酯 | 97.4% | 97.2% | 104.7% | ||||||||
56 | o,p'-DDE | 104.4% | 107.1% | 103.3% | 113 | 苯醚甲环唑 | 94.6% | 89.8% | 92.0% | ||||||||
57 | 乙基溴硫磷 | 87.1% | 87.6% | 90.5% |
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