Quantitative determination of glufosinate in biological samples by liquid chromatography with ultraviolet detection after p-nitrobenzoyl derivatization.
We have established a new HPLC method for derivatizing and quantifying glufosinate (GLUF) in human serum and urine using p-nitrobenzoyl chloride (PNBC). The p-nitrobenzoyl derivative of GLUF (PNB-GLUF) was produced quantitatively over 10 min at room temperature. PNB-GLUF possesses the property of ultraviolet (UV) light absorption with a lambda(max) of 272.8 nm, and was isolated from biological specimens by reversed-phase chromatography using Inertsil Ph-3. In experiments at a UV wavelength of 273 nm, GLUF has a quantitative detection limit of 0.005 microg/ml, and when it was added to both serum and urine to yield concentrations of 0.1-1000 microg/ml, its recovery rate was quite satisfactory: at least 93.8% in all cases. Further, the measured amounts of GLUF in 23 serum samples from patients intoxicated by ingestion of GLUF compared favorably with those obtained by fluorescence derivatization-HPLC using 9-fluorenylmethyl chloroformate (R=0.998). This technique of analysis is, in addition, applicable for Glyphosat, which possesses a chemical structure resembling that of GLUF, and it will be of great use in the determination of these two compounds.
蛍光検出-高速液体クロマトグラフィーによるDL-ホモアラニン-4-イル(メチル)ホスフィン酸の迅速定量
毒性が低くはん用性の高い除草剤である,DL-ホモアラニン-4-イル(メチル)ホスフィン酸(グルホシネート)の高速液体クロマトグラフ装置を用いた迅速分析法について検討した.高感度定量を行うため,アミノ酸分析に用いられている9-フルオレニルメチルクロロホルメート(FMOC-Cl)を用いてグルホシネートを蛍光ラベル化した.蛍光ラベル化は,試料溶液にpH8.5のホウ酸緩衝溶液と0.1%FMOC-Clアセトン溶液を加え,40℃で10分間加温する.反応終了後,未反応試薬を除去し,蛍光検出器付き高速液体クロマトグラフ装置で分析した.カラムとしては最もはん用性の高いオクタデシルシリルカラムを,移動相にはアセトニトリル-リン酸緩衝溶液(pH2.5)系を用いた.生成した誘導体は19時間経過しても安定であった.検量線は0.2～20.0μgcm-3の範囲で良好な直線を示し,その相関係数は0.99で,検出限界は1ngcm-3であった.生体試料に応用するため,前処理法について検討したところ,あらかじめ試料をpH8.5のホウ酸緩衝溶液で希釈した後,アセトンで除タンパクする方法が最良で,グルホシネートの回収は定量的であった.グルホシネートを含む製剤を嚥下したヒト血液,尿について分析したところ,共存成分による妨害も見られず,1検体当たり40分足らずで容易に定量可能であった.
From the World Literature
LIST OF ILLUSTRATIONS ix ACKNOWLEDGMENTS xi INTRODUCTION: Goethe Coins a Phrase 1 PART ONE: CIRCULATION Chapter 1: Gilgamesh's Quest 39 Chapter 2: The Pope's Blowgun 78 Chapter 3: From the Old World to the Whole World 110 PART TWO: TRANSLATION Chapter 4: Love in the Necropolis 147 Chapter 5: The Afterlife of Mechthild von Magdeburg 170 Chapter 6: Kafka Comes Home 187 PART THREE: PRODUCTION Chapter 7: English in the World 209 Chapter 8: Rigoberta Menchu in Print 231 Chapter 9: The Poisoned Book 260 CONCLUSION: World Enough and Time 281 BIBLIOGRAPHY 305 INDEX 319