| UHPLC－MS/MS法分析氯化乙酰甲胆碱雾化气溶胶浓度 |
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| 基金项目:浙江省自然科学基金项目（LY17H310004） |
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| 中文摘要:建立了超高效液相色谱－三重四极杆质谱（UHPLC－MS/MS）测定吸入雾化装置中氯化乙酰甲胆碱气溶 胶药物浓度的方法。采用ACQUITY BEH C18（2. 1 mm × 100 mm，1. 7 μm）色谱柱，以0. 1%甲酸水和乙腈作为流 动相梯度洗脱，流速为0. 3 mL/min，进样量为5 μL，分析时间为5 min，柱温为40 ℃，多反应监测（MRM）正离 子模式测定。同时，对专属性、线性、仪器精密度、加标回收率、提取回收率和稳定性分别进行了考察。结果 表明，氯化乙酰甲胆碱在10～100 ng/mL质量浓度范围内线性良好（r ＞ 0. 999），定量下限为10 ng/mL；氯化乙 酰甲胆碱雾化气溶胶的平均加标回收率为99. 2%，平均相对标准偏差（RSD）为0. 80%；雾化气溶胶的平均提取 回收率为95. 7%。在吸入暴露装置中雾化1 min后，气溶胶的平均药物浓度为608. 1 mg/m3 ，上、中、下位置的 RSD为1. 2%，表明雾化1 min氯化乙酰甲胆碱气溶胶浓度即达到均一。该方法灵敏度高，精密度好，适用于氯 化乙酰甲胆碱雾化气溶胶的浓度测定，也可为吸入制剂雾化气溶胶供试品分析提供参考。 |
| 中文关键词:超高效液相色谱－串联质谱法 氯化乙酰甲胆碱 雾化气溶胶 吸入制剂 |
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| Quantification of Aerosol Content of Metha? choline Chloride Powder by UHPLC－MS/ MS |
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| Abstract:An ultra-high performance liquid chromatography－tandem mass spectrometric（UHPLC－ MS/MS）method was established for the determination of aerosol content of methacholine chloride for inhalation solution. The sample was separated on an ACQUITY BEH C18（2. 1 mm × 100 mm， 1. 7 μm）column by gradient elution，using 0. 1% formic acid water and acetonitrile as the mobile phases with a flow rate of 0. 3 mL/min，an injection volume of 5 μL，an analysis time of 5 min and a column temperature of 40 ℃，and finally determined in multiple-reaction monitoring（MRM）mode. Meanwhile，the specificity，linearity，instrument precision，spiked recovery，extraction recovery and stability were investigated. Methacholine chloride was linear in the range of 10－100 ng/mL（r ＞ 0. 999）. The limit of quantitation was 10 ng/mL. The recovery for methacholine chloride in aerosols was 99. 2% with a relative standard deviation（RSD）of 0. 80%. The extraction efficiency for methacho? line chloride was 95. 7%. After atomizated for 1 min in the inhalation exposure device，the average content of methacholine chloride in the aerosols was 608. 1 mg/m3 . RSD of the upper，middle and low? er positions was 1. 2%. It indicated that the content of methacholine chloride in the aerosols was uni? form after 1 min atomization. The method is sensitive and precise，and is suitable for the determina? tion of aerosol content of methacholine chloride powder for inhalation solution，and it also could be used as a reference for the analysis of other aerosol samples for inhalation. |
| Key Words:ultra-high performance liquid chromatography－tandem mass spectrometry ?methacholine chloride ?atomization aerosol ?inhalation |
| 引用本文：朱狄峰，赵剑岚，洪雅雯，钱仁云，陈 超，平 丽.UHPLC－MS/MS法分析氯化乙酰甲胆碱雾化气溶胶浓度[J].分析测试学报,2021,40(8):1145-1150. |
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