| 第 51 卷第 6 期 |  | Vol. 51 No. 6 | | 2021 年 12 月 | Dec 2021 |
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所屬欄目：分析與測試
HPLC 法測定伐地昔布的有關(guān)物質(zhì) |
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千 夢(mèng) ， 張 云 ， 孫 玲 ＊， 王 金 虎
（山東省藥學(xué)科學(xué)院， 山東省化學(xué)藥物重點(diǎn)實(shí)驗室， 山東 濟南 250101)
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| 摘 要：建立高效液相色譜法檢測伐地昔布的有關(guān)物質(zhì)。 采用 儀一酸性糖蛋白鍵合硅膠的手性色譜柱， 以
乙睛一醋酸綏緩沖液 （0.01 mol / L， pH4.0） 作為流動(dòng)相進(jìn)行梯度洗脫， 檢測波長(cháng) 215 nm。 伐地昔布與 5 個(gè)已知雜質(zhì)均可達到基線(xiàn)分離， 在各自濃度范圍內線(xiàn)性關(guān)系良好，
平均回收率 95.13%-99.77%， RSD1.10%-
1.77%， 檢測限 0.017 9-0.060 1 μg / mL， 定量限 0.059 7-0.200 0 μg / mL。 方法專(zhuān)屬性強， 準確度好， 靈敏度高，
可為伐地昔布的質(zhì)量控制及后續分離提純和帕瑞昔布的質(zhì)量控制提供指導。
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| 關(guān)鍵詞：
帕瑞昔布； 伐地昔布； 高效夜相色譜法； 有關(guān)物質(zhì)； 質(zhì)量控制
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| 中圖分類(lèi)號：0657.7 文獻標識碼：A 文章編號：1009-9212(2021)06-0077-05 |
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Determination of Related Substances in Valdecoxib by HPLC
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YU Meng ZHANG Yun SUN Ling＊ WANG Jin-hu
( Shandong Academy of Pharmaceutical Sciences, Shandong Provincial Key Laboratory of Chemical Drug,
Jinan 250101, China)
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| Abstract：To establish a HPLC method for the determination of the related substances in valdecoxib,
a chira chromatography column packed with a-acid glycoprotein-bonded silica gel was used, and
acetonitrile-ammoniu acetate buffer (0.01 mol/L, pH4.0) was used as the mobile phase for gradient
elution, and the detection wavelengt was set at 215 nm. Valdecoxib and five known impurities could
achieve a baseline separation, and the linea
relationship was good within their respective concentration ranges; the average recovery rate was
95.13%-99.77%
and the RSD was 1.10%-1.77%; the limit of detection was 0.017 9-0.060 1 μ,g/mL; the limit of
quantification wa
0.059 7 -0.200 0 μ,g/mL. This method has good specificity, high accuracy and sensitivity, which can
provid guidance for the quality control of valdecoxib, as well as the subsequent separation and
purification and qualit
control of parecoxib.
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| Key words：
parecoxib; valdecoxib; HPLC; related substances; quality control
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作者簡(jiǎn)介：
于 夢(mèng)（1988—)，女，山東菏澤人，主管藥師，主要從事藥物研發(fā)質(zhì)掀控制（E-mail yumengsdaps@163.com)。
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聯(lián) 系 人：孫 玲，主任藥師，主要從事中藥、化藥新藥質(zhì)量研究工作（工-mail Sunl_70@126.com）
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收稿日期：2021-09-16
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