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LC/MS (TOF) Analysis of Drugs and Their Glucuronide Metabolites in Urine on Titan C18 after Solid Phase Extraction (SPE) using Supel™-Select SCX, β-Glucuronidase Enzyme Digestion

LC/MS (TOF) Analysis of Drugs and Their Glucuronide Metabolites in Urine on Titan C18 after Solid Phase Extraction (SPE) using Supel™-Select SCX, β-Glucuronidase Enzyme Digestion application for HPLC, application for SPE

材料

SPEチューブまたはプレート

製品番号
詳細
価格

54241-U

Supel™-Select SCX SPE チューブ

bed wt. 60 mg, volume 3 mL, pk of 50

標準

製品番号
詳細
価格

C-006

Codeine solution

1 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

O-902

オキサゼパム 溶液

1 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

H-004

Hydromorphone solution

1 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

B-044

ブプレノルフィン 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

H-003

ヒドロコドン 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

L-901

ロラゼパム 溶液

1.0 mg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®

M-005

モルヒネ 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

N-059

ノルブプレノルフィン 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

O-004

Oxymorphone solution

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

T-019

(−)-11-ノル-9-カルボキシ-Δ9-THC 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

T-037

テストステロン 溶液

1.0 mg/mL in acetonitrile, ampule of 1 mL, certified reference material, Cerilliant®

T-058

Tapentadol hydrochloride solution

1.0 mg/mL in methanol (as free base), ampule of 1 mL, certified reference material, Cerilliant®

T-907

テマゼパム 溶液

1.0 mg/mL in methanol, ampule of 1 mL, certified reference material, Cerilliant®

酵素

製品番号
詳細
価格

G2174

β-グルクロニダーゼ カサガイ（Patella vulgata）由来

aqueous solution, ≥85,000 units/mL

CONDITIONS

sample preparation

Solid Phase Extraction (SPE)

sample/matrix

human urine

SPE tube/cartridge

Supel-Select SCX, 60 mg/3 mL (54241-U)

extraction process

urine samples were spiked at 200 ng/mL each analyte and digested with 10kU of beta-glucuronidase enzyme at 60 °C for 120 min

condition

1 mL of 1% formic acid in acetonitrile followed by 1 mL water

sample addition

1.4 mL urine

washing

2 mL water followed by 1 mL of water:methanol (75:25)

elution

1 mL of 10% ammonium hydroxide in acetonitrile

eluate post-treatment

evaporate to dryness and reconstitute in 1 mL water

column

Titan C18, 5 cm x 2.1 mm I.D., 1.9 μm particles (577122-u)

mobile phase

[A] 5 mM ammonium formate; [B] 5 mM ammonium formate in acetonitrile:water (95:5)

gradient

5 to 90% B in 2.5 min, held for 0.5 min, to 5% B in 0.1 min, held for 0.5 min

flow rate

0.3 mL/min

column temp.

35 °C

detector

ESI(+) TOF, m/z 100-1000

injection

2 μL

詳細

アナリシスノート

A set of compounds representing five drug classes that are routinely tested in urine were extracted from urine and analyzed using LC/MS (TOF). The entire workflow, from enzymatic digestion to hydrolyze the glucuronide metabolites to analysis using a Titan UHPLC column is presented here. Cerilliant CRMS provided reliable quantification.
Sample pretreatment: urine samples were spiked at 200 ng/mL each analyte and digested with 10kU of beta-glucuronidase enzyme at 60 °C for 120 min

法的情報

Supel is a trademark of Sigma-Aldrich Co. LLC
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