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Accuracy Profile Theory for the Validation of an LC–MS-MS Method for the Determination of Risperidone and 9-Hydroxyrisperidone in Human Plasma

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Abstract

A sensitive and specific LC–MS-MS method is described for the simultaneous quantification of risperidone and 9-hydroxyrisperidone in human plasma. After extraction with tert-butyl methyl ether, plasma samples were separated on an Atlantis HILIC Silica C18 column (4.6 × 150 mm, 5 μm)with a mobile phase of ammonium formate buffer (10 mM, pH 4.0)/acetonitrile (40/60, v/v). Detection was by MS-MS. The method was fully validated according to the accuracy profile theory. It is based on β-expectation tolerance interval for the total measurement error which includes trueness and intermediate precision. The measurement uncertainty derived from β-expectation tolerance interval was estimated at each of the validation standards. The linearity fitted well over the range of 0.11–26.75 ng mL−1 for risperidone with an LLOQ of 0.11 ng mL−1, and for 9-hydroxyrisperidone, at a range of 0.15–37.8 ng mL−1 with an LLOQ of 0.15 ng mL−1. The intra- and inter-batch precision of risperidone were <5.71 and 8.22%, respectively. For 9-hydroxyrisperidone, the data were 5.78 and 6.48%. The recoveries were 88.78% (risperidone) and 70.35% (9-hydroxyrisperidone). The developed method was applied to a pharmacokinetic study of risperidone.

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Authors and Affiliations

  1. Department of Pharmacy, Peking University Third Hospital, Beijing, 100191, People’s Republic of China

    Xianhua Zhang, Chao Zhang, Li Yang, Xin Xiong, Yong Zhou, Yiheng Yang & Jingli Duan

  2. Department of Pharmacy, Peking University First Hospital, Beijing, 100034, People’s Republic of China

    Xia Zhao

Authors
  1. Xianhua Zhang
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  2. Xia Zhao
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  3. Chao Zhang
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  4. Li Yang
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  5. Xin Xiong
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  6. Yong Zhou
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  7. Yiheng Yang
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  8. Jingli Duan
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Correspondence to Jingli Duan.

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Zhang, X., Zhao, X., Zhang, C. et al. Accuracy Profile Theory for the Validation of an LC–MS-MS Method for the Determination of Risperidone and 9-Hydroxyrisperidone in Human Plasma. Chroma 71, 1015–1023 (2010). https://doi.org/10.1365/s10337-010-1580-3

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