Determination of Contents of Monoester Alkaloids and Limit Test of Diester Alkaloids in Fupian (Heishunpian) Formula Granules by HPLC

doi:10.19803/j.1672-8629.20260284

Abstract

Abstract: Objective To establish a high performance liquid chromatography (HPLC) method for simultaneous determination of three monoester alkaloids and for the limit test of three diester alkaloids so as to offer a feasible detection approach to quality control of related samples. Methods Using Fupian (Heishunpian) formula granules as the subject, the contents of three monoester alkaloids and three diester alkaloids were determined by HPLC-tandem mass spectrometry (HPLC-MS/MS) before an HPLC method was established to determine the contents of the three monoester alkaloids, the limit test of diester alkaloids and those of multiple batches of samples of Fupian (Heishunpian) formula granules. Results The HPLC-MS/MS results showed that 1 g of the test sample contained a total of 1.5 mg of monoester alkaloids and a total of 2.5 μg of diester alkaloids, which met the national standard. Using the established HPLC method, the three monoester alkaloids were highly linear within the range of tested concentrations (correlation coefficient R²>0.999), The total content of monoester alkaloid in 1 g of Fupian (Heishunpian) formula granules was 1.3 mg·g^-1, and no diester alkaloids were detected. Based on the instrumental quantitation limit and the national standard limit, the contents of diester alkaloids were believed to comply with the limit requirement. In multiple batches of samples detected by HPLC, the contents of monoester alkaloids all met the related standard and no diester alkaloids were detected. Conclusion The HPLC method established in this study is user-friendly and has excellent universality. Within the linear range, it can be used for the determination of monoester alkaloids and the limit test of diester alkaloids in Fupian (Heishunpian) formula granules as a complementary detection approach.

Key words: Fupian (Heishunpian) Formula Granules, Monoester Alkaloids, Diester Alkaloids, High Performance Liquid Chromatography (HPLC) Method, Liquid Chromatography-Tandem Mass Spectrometry (LC-MS), Alkaloid Determination

CLC Number:

R282
R927

WANG Minshu, CHENG Ding, WU Chengfeng, ZHANG Chunyan, YANG Yuqin, ZHANG Zhiguo. Determination of Contents of Monoester Alkaloids and Limit Test of Diester Alkaloids in Fupian (Heishunpian) Formula Granules by HPLC[J]. Chinese Journal of Pharmacovigilance, 2026, 23(6): 643-648.

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https://zgywjj.magtechjournal.com/EN/Y2026/V23/I6/643

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