手性NACE法测定富马酸福莫特罗粉吸入剂中富马酸福莫特罗对映体的含量

张修齐; 张波; 苏靓丽; 陈春雨; 王利娟; 乔晓强

doi:10.13748/j.cnki.issn1007-7693.20232815

手性NACE法测定富马酸福莫特罗粉吸入剂中富马酸福莫特罗对映体的含量

Content Determination of the Enantiomers of Formoterol Fumarate in Formoterol Fumarate Powder Inhaler by Chiral NACE

摘要

摘要:
目的以L(+)-酒石酸–硼酸络合酸为手性选择剂，建立手性非水毛细管电泳法，对富马酸福莫特罗(formoterol fumarate，FMT·FUM)进行手性分离，并测定FMT·FUM粉吸入剂中对映体的含量。
方法以未涂层熔融弹性石英毛细管(65 cm×50 μm，45.0 cm)为分离通道；运行电压20 kV；检测波长214 nm；室温；优化的背景缓冲液为含40 mmol·L⁻¹ L(+)-酒石酸、400 mmol·L⁻¹硼酸、0.4%三乙胺的甲醇溶液。
结果 FMT·FUM的2个对映体在优化的手性分离条件下能够被完全分离，分离度为9.5；出峰顺序为RR-FMT·FUM在前，SS-FMT·FUM在后；在2.5~250.0 μg·mL⁻¹，2个对映体的质量浓度与峰面积分别呈现良好的线性关系；RR-FMT·FUM和SS-FMT·FUM的加标回收率在99.2%~101.8%，相对标准偏差为1.0%~1.9%，表明该法准确度良好；RR-FMT·FUM和SS-FMT·FUM的标示量百分含量分别为98.5%和99.1%，相对标准偏差分别为1.3%和1.5%。
结论此方法可用于FMT·FUM粉吸入剂中对映体的含量测定。

Abstract:
OBJECTIVE To establish a chiral nonaqueous capillary electrophoresis(NACE) method, L(+)-tartaric acid–boric acid complex was used as the chiral selector for the chiral separation of formoterol fumarate(FMT·FUM) and determination of the enantiomers of FMT·FUM in FMT·FUM powder inhaler.
METHODS An uncoated fused silica capillary(65 cm × 50 μm, 45.0 cm) was used as the separation channel, along with the applied voltage of 20 kV, detection wavelength of 214 nm, room temperature. The optimized background buffer was the methanol solution containing 40 mmol·L⁻¹ L(+)-tartaric acid, 400 mmol·L⁻¹ boric acid, and 0.4% triethylamine.
RESULTS The two enantiomers of FMT·FUM could be completely separated under the optimized chiral separation conditions, and the Rs was 9.5. The migration order was the former RR-FMT·FUM and the later SS-FMT·FUM. Good linearity of the peak area for the two enantiomers were showed in the concentration range of 2.5–250.0 μg·mL⁻¹, respectively. The recoveries of RR-FMT·FUM and SS-FMT·FUM were 99.2%–101.8%, with relative standard deviations(RSDs) of 1.0%–1.9%, indicating good accuracy of the method. The percentage of labeled quantities were 98.5% and 99.1% for RR-FMT·FUM and SS-FMT·FUM, with RSDs of 1.3% and 1.5%, respectively.
CONCLUSION The method is suitable for the determination of the enantiomer contents in FMT·FUM powder inhaler.

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