HPLC enantioseparation of α,α-diphenyl-2-pyrrolidinemethanol and methylphenidate using a chiral fluorescent derivatization reagent and its application to the analysis of rat plasma.
HPLC enantioseparation of α,α-diphenyl-2-pyrrolidinemethanol and methylphenidate using a chiral fluorescent derivatization reagent and its application to the analysis of rat plasma.
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使用手性荧光衍生试剂对 α,α-二苯基-2-吡咯烷甲醇和哌醋甲酯进行 HPLC 对映分离及其在大鼠血浆分析中的应用。
DOI：
10.1002/jssc.201000479
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发表时间：
2010
影响因子：
3.1
通讯作者：
T. Toyo′oka
中科院分区：
文献类型：
--
作者：
Shinsuke Inagaki;Sayuri Taniguchi;Haruo Hirashima;T. Higashi;J. Min;R. Kikura;Y. Goda;T. Toyo′oka
使用 (R)-(-)-4-(N,N-二甲基氨基磺酰基)-7-(3-异硫氰酸吡咯烷-1-基)-2,1,3-苯并恶二唑作为对映体分离 α,α-二苯基-2-吡咯烷甲醇 (D2PM) 和哌甲酯（MPH；利他林(®)） 首次实现了手性衍生化试剂，并开发了一种简单、可靠的高效液相色谱荧光检测方法。 D2PM 和 MPH 已用 (R)-(-)-4-(N,N-二甲基氨基磺酰基)-7-(3-异硫氰酸吡咯烷-1-基)-2,1,3-苯并恶二唑在 55°C 下衍生化 15 分钟。 D2PM 和 MPH 的衍生物已使用反相系统在 16 分钟内完全、快速地分离（分辨率因子 (R(s)) 分别为 1.60 和 2.53）。 (R)-和(S)-D2PM 的检测限分别为 6.8 和 13 ng/mL，D-和 L-threo-MPH 的检测限分别为 61 和 66 ng/mL (S/N=3)。该方法成功应用于大鼠血浆分析，其中大鼠分别服用 D2PM 和 MPH（利他林）。
Enantioseparation of α,α-diphenyl-2-pyrrolidinemethanol (D2PM) and methylphenidate (MPH; Ritalin(®)) using (R)-(-)-4-(N,N-dimethylaminosulfonyl)-7-(3-isothiocyanatopyrrolidin-1-yl)-2,1,3-benzoxadiazole as the chiral derivatization reagent has been achieved for the first time, and a simple, reliable detection method using HPLC with fluorescence detection has been developed. D2PM and MPH have been derivatized with (R)-(-)-4-(N,N-dimethylaminosulfonyl)-7-(3-isothiocyanatopyrrolidin-1-yl)-2,1,3-benzoxadiazole at 55°C for 15 min. The derivatives of D2PM and MPH have been separated, completely and rapidly, using a reversed-phase system within 16 min (resolution factor (R(s))=1.60 and 2.53, respectively). The detection limits of (R)- and (S)-D2PM were found to be 6.8 and 13 ng/mL, respectively, and those of D- and L-threo-MPH were 61 and 66 ng/mL, respectively (S/N=3). The proposed method was successfully applied to the analysis of rat plasma, where the rats were separately dosed with D2PM and MPH (Ritalin).