植物源性食品中46种农药多残留的分析方法
? 样品前处理方法
? 仪器分析方法
仪器:岛津GCMS-TQ 8030气质联用仪 | 载气:氦气 |
色谱柱:Rtx-5MS,30 m×0.25 mm×0.25 μm | 载气流速:1 mL/min |
柱温: | 碰撞气:氩气 |
进样口温度:250oC | 进样方式:不分流进样(1 min) |
接口温度:250oC | 进样量:1 μL |
离子源温度:250oC | 检测模式:多反应监测(MRM) |
? 结果
将空白样品(苹果、茄子、绿茶、大米)添加0.05 mg/kg的46种农药后,按上述前处理及仪器分析方法,使用对应的维泰克QuEChERS试剂包,采用基质匹配的校准曲线,平行三份样品考察添加回收率和相对标准偏差(RSD),结果如下表所示,46种农药的加标回收率在72.5-120.6%之间,相对标准偏差小于14.2%。
编号 | 农药 | 苹果 | 茄子 | 绿茶 | 大米 | ||||
回收率 (%) | RSD (%) | 回收率 (%) | RSD (%) | 回收率(%) | RSD (%) | 回收率(%) | RSD (%) | ||
1 | 敌敌畏 | 78.2 | 8.7 | 80.3 | 9.2 | 76.5 | 6.2 | 74.3 | 8.2 |
2 | 甲拌磷 | 95.6 | 6.3 | 102.5 | 4.2 | 82.3 | 6.8 | 92.5 | 8.5 |
3 | alpha-六六六 | 105.3 | 6.5 | 85.2 | 2.1 | 92.5 | 9.2 | 82.8 | 3.2 |
4 | 乐果 | 102.5 | 8.2 | 80.8 | 10.2 | 97.5 | 8.9 | 83.7 | 12.1 |
5 | beta-六六六 | 115.6 | 7.8 | 112.3 | 13.2 | 92.7 | 6.4 | 108.2 | 9.5 |
6 | gamma-六六六 | 105.8 | 9.9 | 88.3 | 5.6 | 73.2 | 8.6 | 97.5 | 6.9 |
7 | 五氯硝基苯 | 96.3 | 11.2 | 105.8 | 3.9 | 72.5 | 3.2 | 89.2 | 9.5 |
8 | 嘧霉胺 | 89.6 | 5.9 | 112.4 | 5.9 | 98.2 | 4.3 | 115.2 | 1.4 |
9 | 二嗪磷 | 97.5 | 6.2 | 120.3 | 11.7 | 113.6 | 6.9 | 90.3 | 7.3 |
10 | 乙烯菌核利 | 108.6 | 7.8 | 95.4 | 10.2 | 109.0 | 1.5 | 90.2 | 5.3 |
11 | 甲基对硫磷 | 110.2 | 8.9 | 89.9 | 8.4 | 101.2 | 6.2 | 109.4 | 2.1 |
12 | 杀螟硫磷 | 94.5 | 4.3 | 88.4 | 9.2 | 89.3 | 7.4 | 107.2 | 3.2 |
13 | 马拉硫磷 | 107.8 | 2.1 | 109.2 | 2.8 | 90.2 | 9.3 | 98.2 | 6.3 |
14 | 91.5 | 9.1 | 117.2 | 8.2 | 112.5 | 4.2 | 109.0 | 8.4 | |
15 | 毒死蜱 | 89.2 | 3.1 | 86.4 | 3.4 | 105.8 | 6.1 | 90.2 | 3.2 |
16 | 对硫磷 | 94.5 | 4.2 | 89.6 | 6.2 | 117.8 | 8.5 | 88.3 | 4.1 |
17 | 三氯杀螨醇 | 88.2 | 5.2 | 107.7 | 5.4 | 108.2 | 7.3 | 78.9 | 7.2 |
18 | 三唑酮 | 103.8 | 8.2 | 111.4 | 6.1 | 107.6 | 3.8 | 87.3 | 8.3 |
19 | 水胺硫磷 | 109.2 | 9.2 | 104.2 | 4.2 | 94.3 | 9.3 | 112.7 | 7.3 |
20 | 甲基异柳磷 | 90.9 | 8.6 | 109.2 | 5.2 | 101.2 | 8.5 | 114.3 | 8.2 |
21 | 二甲戊乐灵 | 89.7 | 10.2 | 111.4 | 7.1 | 84.3 | 5.3 | 97.4 | 6.3 |
22 | 氟虫腈 | 96.7 | 3.2 | 107.1 | 3.5 | 83.5 | 2.1 | 95.2 | 3.0 |
23 | 腐霉利 | 104.6 | 4.3 | 94.9 | 4.5 | 112.3 | 4.2 | 103.2 | 6.6 |
24 | 丙溴磷 | 104.1 | 2.8 | 107.0 | 4.2 | 95.7 | 5.0 | 85.7 | 4.1 |
25 | p,p'-DDE | 107.4 | 1.4 | 86.8 | 1.1 | 84.3 | 1.5 | 97.0 | 0.9 |
26 | 虫螨腈 | 88.6 | 7.0 | 90.5 | 6.8 | 94.3 | 4.6 | 106.3 | 9.8 |
27 | p,p'-DDD | 101.4 | 3.6 | 108.2 | 4.8 | 97.3 | 5.5 | 78.4 | 1.8 |
28 | o,p'-DDT | 111.1 | 5.7 | 107.6 | 2.1 | 102.2 | 5.4 | 116.0 | 5.6 |
29 | 三唑磷 | 109.2 | 1.0 | 88.8 | 5.0 | 96.8 | 4.7 | 89.0 | 4.4 |
30 | p,p'-DDT | 113.0 | 6.1 | 96.8 | 2.4 | 98.4 | 3.1 | 85.1 | 1.0 |
31 | 异菌脲 | 89.3 | 6.0 | 89.7 | 2.2 | 95.8 | 4.2 | 110.8 | 4.7 |
32 | 联苯菊酯 | 112.0 | 10.0 | 105.4 | 3.7 | 105.8 | 6.1 | 96.4 | 3.3 |
33 | 亚胺硫磷 | 105.5 | 6.7 | 89.2 | 3.6 | 94.7 | 5.3 | 108.8 | 4.1 |
34 | 甲氰菊酯 | 74.9 | 10.3 | 80.5 | 3.9 | 87.7 | 3.4 | 101.8 | 12.9 |
35 | 伏杀硫磷 | 110.2 | 5.2 | 91.8 | 2.9 | 101.2 | 6.0 | 106.4 | 12.4 |
36 | 哒螨灵 | 97.2 | 4.2 | 91.4 | 2.3 | 95.2 | 5.7 | 106.0 | 7.2 |
37 | 嘧菌酯 | 107.5 | 4.2 | 103.8 | 3.9 | 99.3 | 6.5 | 115.7 | 5.8 |
38 | 氯氟氰菊酯 | 107.2 | 5.9 | 107.7 | 3.3 | 95.3 | 7.1 | 120.6 | 8.9 |
39 | 氯菊酯 | 83.8 | 4.7 | 109.8 | 3.2 | 91.8 | 6.0 | 101.8 | 9.1 |
40 | 氟氯氰菊酯 | 106.4 | 5.7 | 84.1 | 6.8 | 90.9 | 6.9 | 112.8 | 9.7 |
41 | 氯氰菊酯 | 74.1 | 9.0 | 83.6 | 4.6 | 81.5 | 3.4 | 98.5 | 14.2 |
42 | 氟氰戊菊酯 | 85.0 | 3.8 | 83.2 | 3.2 | 80.6 | 3.2 | 104.2 | 7.6 |
43 | 氰戊菊酯 | 81.8 | 8.7 | 74.0 | 3.9 | 81.9 | 3.3 | 105.9 | 7.9 |
44 | 氟胺氰菊酯 | 98.9 | 2.8 | 73.2 | 4.8 | 83.5 | 5.6 | 103.5 | 8.7 |
45 | 苯醚甲环唑 | 88.6 | 9.3 | 80.3 | 4.7 | 96.0 | 3.6 | 115.8 | 10.6 |
46 | 溴氰菊酯 | 84.8 | 5.5 | 75.5 | 6.6 | 72.5 | 2.9 | 96.3 | 4.7 |
维泰克QuEChERS产品订货信息
样品基质 | 样品量 | 提取溶剂 | 提取包 | 净化管 | |
EN方法 | 蔬菜、水果、食用菌 (颜色较浅的样品,如番茄、苹果、土豆、梨、甘蓝等) | 10.0 g | 10 mL乙腈 | 4g MgSO4 1gNaCl 1g柠檬酸钠 0.5g 柠檬酸氢二钠 盐包:WQ-MN40115N | 150 mg PSA 900 mg MgSO4 |
蔬菜、水果、食用菌 (颜色较深的样品,如茄子、豆角、韭菜、芹菜等) | 10.0 g | 10 mL乙腈 | 4g MgSO4 1gNaCl 1g柠檬酸钠 0.5g 柠檬酸氢二钠 盐包:WQ-MN40115N | 150 mg PSA 15 mg GCB 885 mg MgSO4 | |
AOAC方法 | 茶叶、香辛料 | 2.0 g+10 mL水 | 15 mL乙腈(含1%乙酸) | 6g MgSO4 1.5g NaOAc 盐包:WQ-MN40115N | 400 mg PSA 400 mg C18 200 mg GCB 1200 mg MgSO4 |
谷物、油料、坚果 | 5.0 g+10 mL水 | 15 mL乙腈(含1%乙酸) | 6g MgSO4 1.5g NaOAc 盐包:WQ-MN40115N | 400 mg PSA 400 mg C18 1200 mg MgSO4 |