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| Quantification of Aerosol Content of Metha? choline Chloride Powder by UHPLC－MS/ MS |
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| DOI： |
| KeyWord:ultra-high performance liquid chromatography－tandem mass spectrometry ?methacholine chloride ?atomization aerosol ?inhalation |
| Author | Institution |
| ZHU Di-feng， ZHAO Jian-lan， HONG Ya-wen， QIAN Ren-yun，CHEN Chao，PING Li |
Center for Drug Safety Evaluation and Research，College of Pharmaceutical Sciences，Zhejiang University， Hangzhou ，China |
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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. |
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