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LC/MS/MS Analysis of Neonicotinoid Pesticides in Dandelion Blossoms on Ascentis® Express C18 after Dispersive SPE (QuEChERS) using Supel QuE

LC/MS/MS Analysis of Neonicotinoid Pesticides in Dandelion Blossoms on Ascentis® Express C18 after Dispersive SPE (QuEChERS) using Supel™ QuE application for HPLC

材料

SPEチューブまたはプレート

製品番号
詳細
価格

Supel QuE

Acetate Tube, pk of 50, AOAC® 2007.01

Supel QuE

Empty Centrifuge Tube with Lid, centrifuge tube volume 50 mL, pk of 50, suitable for EN 15662:2008 per BS

分析カラム

製品番号
詳細
価格

Ascentis® Express C18, 2.7 µm HPLCカラム

2.7 μm particle size, L × I.D. 10 cm × 3 mm

標準

製品番号
詳細
価格

ニテンピラム

PESTANAL®, analytical standard

イミダクロプリド

PESTANAL®, analytical standard

イミダクロプリド 溶液

100 μg/mL in acetonitrile, PESTANAL®, analytical standard

チアクロプリド

PESTANAL®, analytical standard

チアメトキサム

PESTANAL®, analytical standard

N-(6-クロロ-3-ピリジルメチル)-N-シアノ-N-メチルアセタミジン

PESTANAL®, analytical standard

イミダクロプリド-d4

PESTANAL®, analytical standard

クロチアニジン

PESTANAL®, analytical standard

アセタミプリド-D-デスメチル

PESTANAL®, analytical standard

2-イミダゾリドン

PESTANAL®, analytical standard

6-ヒドロキシピリジン-3-カルボン酸

PESTANAL®, analytical standard

6-クロロニコチン酸

PESTANAL®, analytical standard

N-Desmethylthiamethoxam

PESTANAL®, analytical standard

Thiamethoxam-d3

PESTANAL®, analytical standard

Clothianidin-d3

PESTANAL®, analytical standard

Acetamiprid-d3

PESTANAL®, analytical standard

ジノテフラン

PESTANAL®, analytical standard

Desnitro-imidacloprid hydrochloride

PESTANAL®, analytical standard

Thiacloprid-(thiazolidin ring-d4)

PESTANAL®, analytical standard

イミダクロプリド

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

Imidacloprid-olefin

PESTANAL®, analytical standard

チアクロプリド

certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland

移動相成分

製品番号
詳細
価格

アセトニトリル

hypergrade for LC-MS LiChrosolv®

ギ酸

for LC-MS LiChropur

メタノール

hypergrade for LC-MS LiChrosolv®

for chromatography (LC-MS Grade) LiChrosolv®

CONDITIONS

sample preparation

Dispersive (QuEChERS)

sample/matrix

3 g pulverized dandelion blossoms, homogenized in 10 mL water

extraction tube

Supel QuE Acetate extration tube (55234-U)

extraction process

add 25 mL of acetonitrile; add contents of Supel QuE acetate extraction tube; shake immediately for 1 minute; centrifuge at 3400 rpm for 5 minutes

clean-up tube

Supel QuE PSA/C18 tube (55288-U)

clean-up process

Transfer 1 mL of the acetonitrile layer into a Supel QuE PSA/C18 cleanup tube; shake for 1 minute; centrifuge at 3500 rpm for 3 minutes; (draw off 700 uL of supernatant, evaporate to dryness at 50 °C under nitrogen; reconstitute in 200 μL of 50:50 0.1% formic acid:0.1% formic acid in methanol)

column

Ascentis Express C18, 10 cm x 3.0 mm I.D., 2.7 μm particles (53814-U)

mobile phase

[A] 0.1% formic acid in water; [B] 0.1% formic acid in methanol

gradient

30% B from 0 to 5 min; to 100% B in 0.2 min; held at 100% B for 5.3 min; to 30% B in 0.5 min; held at 30% B for 5 min

flow rate

500 μL/min

pressure

3800 psi (262 bar)

column temp.

25 °C

detector

MS, ESI(+), MRM, m/z 203.2/129.2, 271.2/225.0, 292.1/211.0, 256.0/175.2, 250.0/132.0, 223.2/126.0, 253.0/125.8

injection

3 μL

詳細

アナリシスノート

The advent of the die-off of honey bees due to colony collapse disorder (CCD) has spawned investigation into pesticide exposure as the cause. Neonicotinoids are among the suspected culprits. In this application, the QuEChERS approach using Supel QuE was used for extraction and cleanup prior to analysis of seven neonicotinoid pesticides in flower blossoms. Ascentis® Express C18 was chosen due to the high efficiency associated with its Fused-Core® particle, and its relatively low backpressure as compared to sub-2 micron UHPLC columns. This allowed the column to be used in a standard pressure HPLC system with a relatively high concentration of aqueous at the start of the mobile phase gradient.

法的情報

Ascentis is a registered trademark of Merck KGaA, Darmstadt, Germany
Fused-Core is a registered trademark of Advanced Materials Technology, Inc.
Supel is a trademark of Sigma-Aldrich Co. LLC