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7.5分のスクリーニング分析: 玄米粉中の多成分残留農薬

Featured Application: QuEChERS(抽出とクリーンアップ)を使用して玄米粉から抽出された多成分農薬混合物

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分析時間7.5分、分析サイクルは10分以内

200種以上にわたる残留農薬成分の90%以上において70~120%の回収率

汎用HPLCと最新型のUHPLC、どちらの装置にも対応

残留農薬の多成分一斉分析は簡単な仕事ではありません。そして、サンプルマトリックスが複雑であることと日常的に分析に使用するLCMS/MS機器が高度化していることでさらに難しいものになっています。LC-MS/MSを使用することで優れた感度が得られ、ある程度の共溶出があったとしても分析対象物を定量的にモニターできます。しかし、共溶出成分が多すぎると質量分析計の処理性能を超えてしまうため、依然として適切なクロマトグラフィー条件も必須です。ここで示した最適化された条件では分析時間はわずか7.5分、1度の分析サイクルとしては10分以下で、数百の化合物分析を可能とし、高速で正確なサンプルスクリーニングとラボの生産性の向上を確保します。

詳細は次図に示しましたが、玄米粉にRestekのLC Multiresidue Pesticide Kitに含まれるすべての成分を添加したものをサンプルとして、 Q-sep QuEChERS抽出塩で抽出し、dSPEを使用してクリーンアップし、 2.7μm Raptor ARC-18 カラムを使用して分析しました。2.7μmの表面多孔性粒子カラムの特色である効率の良いシャープなピークが得られ、より多くの化合物を所定の時間内に溶出することができます。 また、 Raptor ARC-18 固定相の選択性のため化合物群を分析時間全体にまんべんなく溶出させることができます。これにより特定の時間に多数の化合物の溶出が集中して質量分析計に負荷がかかることを避け、すべての関連イオンを効率的にモニターすることを可能とします。システム容量を最小に保つことが重要であることにもご留意ください。内径の小さなLC配管を選ぶことと過度に長い配管を避けることで、シャープなピークと最速で最も効率的なクロマトグラフィーが得られます。玄米粉中の残留農薬の多成分一斉分析では、質量分析に適したシンプルな移動相と、汎用HPLC装置の運用範囲の背圧を保つ流量を使用しています。この利点により、難しいマトリックスであったとしても、200種以上の農薬、サロゲート化合物、内部標準物質をほんの数分で分析することが可能となります。

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LC_FS0521
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2
1.Cyromazine0.747167.168.143.1
2.Methamidophos1.318142.094.0125.1
3.Formetanate1.681222.1165.046.1
4.Carbofuran1.682222.2165.0123.1
5.Methabenzthiazuron1.686222.0165.0150.0
6.Acephate1.690184.0143.049.0
7.Pymetrozine1.708218.1105.078.0
8.Aminocarb1.716209.1137.1152.1
9.Propamocarb1.735189.1102.0144.1
10.Omethoate1.905214.0125.0183.0
11.Dinotefuran1.972203.1129.187.1
12.Aldicarb sulfoxide2.010207.189.0132.1
13.Butoxycarboxim2.022223.0106.0166.0
14.Nitenpyram2.049271.0225.056.0
15.Aldicarb sulfone2.062240.2148.086.0
16.Carbendazim2.090192.0160.0131.9
17.Oxamyl2.154237.172.090.0
18.Flonicamid2.234230.1203.0148.0
19.Methomyl2.259163.188.0106.1
20.Thiabendazole2.284201.892.2104.0
21.Thiamethoxam2.289292.1211.1181.1
22.Fuberidazole2.368185.0157.1103.0
23.Monocrotophos2.375224.1127.0193.1
24.Mexacarbate2.393223.2166.1151.1
25.Dioxacarb2.397224.1167.077.1
26.Dicrotophos2.526238.1112.172.0
27.Imidacloprid2.536256.1175.0209.0
28.Clothianidin2.545250.0169.0113.0
29.Dimethoate-d6 (IS)2.652236.2205.2131.2
30.Fenuron2.662165.072.146.1
31.Trichlorfon2.667257.0108.9220.8
32.Dimethoate2.668230.0199.0125.0
33.3-Hydroxycarbofuran2.679238.1181.0163.0
34.Vamidothion2.695288.0146.0118.0
35.Mevinphos2.715225.1127.0127.0
36.Acetamiprid2.724223.0126.056.1
37.Propoxur2.777210.0111.0168.0
38.Ethirimol2.780210.2140.298.2
39.Cymoxanil2.805199.1128.2111.2
40.Thiacloprid2.865253.0126.099.0
41.Pirimicarb2.896239.272.0182.1
42.Aldicarb3.022208.2116.289.2
43.Tricyclazole3.066190.0163.0136.0
44.Oxadixyl3.076279.1219.1132.1
45.Carbetamide3.085237.1192.0118.1
46.Simetryn3.122214.168.096.0
47.Thiophanate-methyl3.146343.0151.0311.1
48.Thidiazuron3.150221.1102.1127.9
49.Bendiocarb3.212224.1167.1109.0
50.Imazalil3.225297.1159.041.1
51.Prometon3.227226.1142.1184.0
52.Metribuzin3.230215.1187.1131.0
53.Secbumeton3.232226.2170.2100.2
54.Terbumeton3.235226.1114.1170.1
55.Sulfentrazone*3.263387.0309.0201.0
56.Pyracarbolid3.279218.1125.197.0
57.Tebuthiuron3.310229.1172.1116.0
58.Carbaryl3.316202.1145.0127.0
59.Carboxin3.326236.1143.087.1
60.Monolinuron3.373215.1126.0148.0
61.Fluometuron3.381233.172.146.1
62.Diuron3.382233.172.146.0
63.Ethiofencarb3.406226.0107.0164.0
64.Ametryn3.447228.168.1186.1
65.Chlorotoluron3.450213.072.146.1
66.Metobromuron3.483259.0170.0148.1
67.Propham3.500180.1120.277.1
68.Flutriafol3.508302.070.1123.0
69.Methoprotryne3.532272.1170.0198.1
70.Forchlorfenuron3.536248.1129.093.0
71.Isoprocarb3.537194.195.1137.1
72.Fenpropimorph3.561304.2147.1117.0
73.Atrazine-d5 (SS)3.575221.2179.2101.3
74.Isocarbophos3.606291.1231.1121.1
75.Isoproturon3.612207.172.146.1
76.Desmedipham3.620318.0154.1301.0
77.Phenmedipham3.623318.1108.193.1
78.Spiroxamine3.626298.2144.258.2
79.Pyrimethanil3.659200.0107.082.0
80.Metalaxyl3.691280.1220.1192.1
81.Chlorantraniliprole3.730484.0452.8285.8
82.Cycluron3.785199.189.146.0
83.Prometryn3.830242.1158.0200.2
84.Linuron-d6 (SS)3.843255.1160.1185.2
85.Linuron3.854249.0160.0182.0
86.Thiofanox3.876242.157.2184.0
87.Fenobucarb3.894208.095.1152.1
88.Azoxystrobin3.915404.2329.0344.0
89.Diethofencarb3.924268.1226.1124.0
90.Ethofumesate3.925304.1121.1241.0
91.Ethiprole3.932397.0350.9255.0
92.Fludioxonil*3.935247.1180.1126.1
93.Methiocarb3.958226.1169.1121.1
94.Siduron3.967233.394.0137.1
95.Halofenozide3.974331.1104.9275.0
96.Fenamidone3.993312.092.1236.1
97.Furalaxyl3.995302.1242.195.0
98.Acibenzolar-S-methyl4.023210.9136.191.1
99.Nuarimol4.030315.1252.0207.0
100.Dimethomorph4.044388.2300.9165.1
101.Boscalid4.050343.0306.8140.0
102.Mandipropamid4.067412.1328.1125.0
103.Flutolanil4.079324.1262.0242.0
PeakstR (min)Precursor IonProduct Ion 1Product Ion 2
104.Promecarb4.104208.1109.0151.0
105.Paclobutrazol4.119294.070.1125.0
106.Triadimenol4.119296.170.143.1
107.Mepronil4.161270.191.1119.0
108.Cyproconazole4.175292.270.1125.0
109.Myclobutanil4.195289.270.1125.1
110.Chloroxuron4.225291.172.146.1
111.Bupirimate4.226317.2166.0237.1
112.Methoxyfenozide4.230369.2149.0313.1
113.Triadimefon4.287294.069.0197.0
114.Bifenazate4.290301.1198.0170.1
115.Cyprodinil4.313226.193.077.0
116.Mefenacet4.325299.1148.1120.1
117.Mepanipyrim4.334224.177.1106.1
118.Fluquinconazole4.346376.0348.9307.0
119.Fenhexamid4.383302.197.155.1
120.Fluoxastrobin4.385459.2427.0188.1
121.Tetraconazole4.387372.0159.070.0
122.Bromuconazole isomer 14.392376.0159.0159.0
123.Butafenacil4.411492.1330.9179.9
124.Iprovalicarb4.412321.2119.091.1
125.Flufenacet4.427364.1152.0194.1
126.Triticonazole4.429318.070.0125.0
127.Cyazofamid4.441325.1108.044.0
128.Diflubenzuron4.464311.0158.0141.0
129.Spirotetramat4.478374.1330.1302.0
130.Fenarimol4.510331.0267.9189.1
131.Fenbuconazole4.516337.0125.070.1
132.Epoxiconazole4.529330.0121.1101.0
133.Etaconazole4.552328.1159.055.0
134.Fipronil*4.571436.9332.0252.0
135.Neburon4.635275.057.188.1
136.Flusilazole4.646316.1247.1165.1
137.Fenoxycarb4.653302.288.1116.1
138.Picoxystrobin4.674368.0145.0205.0
139.Rotenone4.683395.1213.1192.1
140.Tebufenozide4.719353.2133.1105.0
141.Dimoxystrobin4.738327.1205.1116.1
142.Bromuconazole isomer 24.740378.0159.0159.0
143.Flubendiamide4.745700.0408.0274.0
144.Diclobutrazol4.764328.070.1159.0
145.Carfentrazone ethyl4.773429.1412.1346.1
146.Kresoxim-methyl4.795314.0267.1116.0
147.Tebuconazole4.827308.070.1124.9
148.Spinosad A4.840732.5142.198.1
149.Penconazole4.853284.170.1159.0
150.Prothioconazole4.857344.0189.0154.0
151.Zoxamide4.893336.1187.0159.0
152.Famoxadone4.933392.2331.1238.0
153.Diazinon-diethyl-d10 (IS)4.961315.2170.2154.3
154.Hydramethylnon4.979495.2323.245.2
155.Triflumuron4.986359.1156.0111.0
156.Prochloraz4.986376.0308.070.1
157.Hexaconazole4.993314.170.0158.8
158.Benalaxyl5.021326.2148.0208.1
159.Metconazole5.033320.170.1125.0
160.Propiconazole5.054342.0159.069.0
161.Pyraclostrobin5.076388.0194.0163.1
162.Clofentezine5.080303.0138.0102.0
163.Bitertanol5.120338.2269.270.1
164.Spinosad D5.142746.5142.098.0
165.Benzoximate5.171364.0199.1105.0
166.Diniconazole5.184326.170.0158.9
167.Thiobencarb5.197258.0125.089.1
168.Pencycuron5.229329.1125.089.0
169.Spinetoram5.234748.5142.198.2
170.Hexaflumuron*5.351459.0439.0175.0
171.Triflumizole5.366346.1278.073.1
172.Indoxacarb5.375528.1149.9203.0
173.Difenoconazole5.380406.1251.1152.0
174.Ipconazole5.426334.270.0124.9
175.Trifloxystrobin5.426409.0186.0206.0
176.Novaluron*5.455491.0471.0304.9
177.Emamectin-benzoate B1b5.463872.2158.282.1
178.Clethodim5.565360.1164.1268.1
179.Teflubenzuron5.614380.9140.9158.0
180.Alanycarb5.636400.191.0238.0
181.Buprofezin5.642306.2106.186.0
182.Emamectin-benzoate B1a5.644886.5158.082.1
183.Benfuracarb5.695411.2194.9251.9
184.Fluazinam*5.726463.0415.9397.9
185.Metaflumizone*5.728505.1302.1328.0
186.Furathiocarb5.735383.1195.0252.1
187.Temephos5.757467.1125.0418.9
188.Lufenuron5.767511.2141.0158.0
189.Tebufenpyrad5.778334.0117.0145.0
190.Pyriproxyfen5.843322.096.0227.1
191.Piperonyl butoxide5.864356.2177.0119.1
192.Hexythiazox5.924353.2228.0168.1
193.Quinoxyfen5.935308.1197.0162.0
194.Flufenoxuron5.984489.1158.0141.0
195.Propargite6.088368.1231.1175.0
196.Etoxazole6.099360.2141.057.1
197.Spiromesifen6.129371.3273.2255.2
198.Chlorfluazuron6.165539.8382.9158.0
199.Spirodiclofen6.269428.371.1313.1
200.(E)-Fenpyroximate6.283422.1366.1138.1
201.Pyridaben6.442365.2147.0309.1
202.Eprinomectin6.466914.6186.1154.1
203.Abamectin B1a6.544890.6305.4567.2
204.Fenazaquin6.559307.1161.0131.1
205.Doramectin6.733916.6331.2593.4
206.Ivermectin6.893892.6551.4569.4
*Detected in ESI- mode
ColumnRaptor ARC-18 (cat.# 9314A12)
Dimensions:100 mm x 2.1 mm ID
Particle Size:2.7 µm
Pore Size:90 Å
Guard Column:Raptor ARC-18 EXP guard column cartridge 5 mm, 2.1 mm ID, 2.7 µm (cat.# 9314A0252)
Temp.:50 °C
Standard/SampleLC multiresidue pesticide kit (cat.# 31971)
Diluent:Water:acetonitrile 9:1
Conc.:1 ng/mL see notes for details
Inj. Vol.:5 µL
Mobile Phase
A:0.2% Formic acid, 2 mM ammonium formate in water
B:0.2% Formic acid, 2 mM ammonium formate in methanol
Time (min)Flow (mL/min)%A%B
0.000.4955
2.000.44060
4.000.42575
6.000.40100
7.500.40100
7.510.4955
9.500.4955
DetectorMS/MS
Ion Mode:ESI+/ESI-
Mode:Scheduled MRM
InstrumentUHPLC
Sample PreparationBrown rice flour (10 g), purchased from a local market, was mixed with 10 mL water. After mixing for 10 min, the brown rice flour was fortified at 10 ng/g with all residues from the LC multiresidue pesticide kit (cat.# 31971), which had been previously combined into a single mixture that day. The fortified brown rice flour suspension was then mixed for 30 min to ensure uniform dispersion of the added pesticide residues in the brown rice flour suspension. Extraction was performed using 10 mL of acetonitrile and original unbuffered QuEChERS salts (cat.# 25848). After centrifugation, 1 mL supernatant was added to a 2 mL dSPE vial containing magnesium sulfate, PSA, and C18 (cat.# 26125) for cleanup. After centrifugation, 100 μL of the 10 ng/mL extract was diluted with 900 μL water and injected onto the UHPLC.
NotesAlthough the ten LC multiresidue pesticides kit mixes are formulated to ensure maximum long-term stability and reliability as packaged, stability may become an issue when a large number of compounds with different chemical functionalities are combined together into a single mix. This should be taken into consideration for quantitative analysis.

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