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目的:利用柱前衍生-反相高效液相色谱法,完善在合成盐酸伪麻黄碱生产过程中的杂质的限度检查,为生产过程的杂质控制提供依据。方法:以(1S)-(+)-氯甲酸薄荷醇酯作为手性衍生化试剂,采用Phenomenex Luna C18柱(250mm×4.6mm,5μm),以乙腈-水-醋酸-三乙胺(29∶20∶0.2∶0.01)为流动相,流速1.0mL·min-1,在254nm处检测。结果:盐酸伪麻黄碱、盐酸左伪麻黄碱、盐酸右麻黄碱、盐酸麻黄碱的浓度均在0.033～0.667μg·mL-1范围内线性关系良好(r>0.99);检测限(S/N=3)分别为56,56,58,56ng;定量限(S/N=10)分别为210,204,226,216ng;各对映体均达到基线分离。结论:方法快速、简便,重复性好,灵敏度高,可用于对合成盐酸伪麻黄碱生产过程中产生的光学异构体进行控制。
OBJECTIVE: To improve the limit of impurities in the synthetic process of pseudoephedrine hydrochloride by pre-column derivatization-RP-HPLC and provide the basis for impurity control in the production process. Methods: Phenomenex Luna C18 column (250 mm × 4.6 mm, 5 μm) was used as chiral derivatization reagent with (1S) - (+) - menthol chloroformate as esterification reagent. 20:0.2:0.01) as the mobile phase at a flow rate of 1.0 mL · min-1 at 254 nm. Results: The linear ranges of pseudoephedrine hydrochloride, pseudoephedrine hydrochloride, dextroamphetamine hydrochloride and ephedrine hydrochloride were all in the range of 0.033-0.667 μg · mL-1 (r> 0.99). The detection limits (S / N = 3) 56, 56, 58 and 56 ng, respectively. The limit of quantification (S / N = 10) was 210, 204, 226 and 216 ng, respectively. Conclusion: The method is rapid, simple, reproducible and sensitive. It can be used to control the optical isomers produced during the synthesis of pseudoephedrine hydrochloride.