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目的:阐明痰热清的化学成分以及痰热清胶囊与痰热清注射液化学成分的差异。方法:采用高效液相色谱法串联质谱(HPLC-ESI-MS/MS)技术,乙腈-0.1%甲酸水为流动相进行梯度洗脱,电喷雾离子源负离子模式下采集数据,并通过准分子离子及二级碎片离子对化学成分进行鉴定。结果:痰热清胶囊中鉴定有机酸类成分7个、黄酮类成分10个、环烯醚萜类成分4个、木脂素类成分3个、苯乙醇苷类成分9个、胆汁酸类成分4个以及未知成分4个等共41个化合物。其中,经由对照品确证化学结构25个,推测化合物结构16个(含4个未知成分)。痰热清注射液中共鉴定化合物23个,相比胶囊注射液中连翘种苷异构体(3个),獐芽菜苷,连翘酯苷B,异连翘酯苷A,连翘酯苷A,芦丁,连翘种苷A异构体(2个),金丝桃苷,aldosecologanin,松脂素-β-D-葡萄糖苷/表松脂素-4’-O-葡萄糖苷/马台树脂醇-4’-O-葡萄糖苷异构体(2个),连翘苷,黄芩素,牛磺鹅去氧胆酸和黄芩提取物中所含的1个未知化合物等18个成分均缺失,可能是注射液无菌生产过程采用活性炭吸附、高温灭菌、配液等工艺以及过程控制中采用超滤技术,从而造成两种制剂化学成分的差异。结论:通过该研究建立的HPLC-ESIMS/MS分析方法,能有效表征痰热清胶囊和痰热清注射液的化学成分差异,可以为两种制剂的质量控制提供依据。
Objective: To elucidate the chemical constituents of Tanreqing and the differences of chemical constituents between Tanreqing Capsule and Tanreqing Injection. Methods: HPLC-ESI-MS / MS, gradient elution with acetonitrile-0.1% formic acid as mobile phase and data acquisition with negative ion mode electrospray ionization And secondary fragment ions to identify the chemical composition. Results: There were 7 organic acids, 10 flavonoids, 4 iridoids, 3 lignans and 3 phenylethanoid glycosides in Tanreqing Capsules. The contents of bile acids 4 and unknown components such as a total of 41 compounds a total of 41. Among them, 25 chemical structures were confirmed through the reference substance, and the structure of the compound was speculated to be 16 (including 4 unknown components). In Tanreqing Injection, 23 compounds were identified. Compared with three kinds of isomers of Forsythiaside (3) in the capsule injection, matrine, forsythiaside B, isoprinoside A, forsythiaside Glycosides A, rutin, forsythiaside A isomers (2), hyperin, aldosecologanin, psoralen-beta-D-glucoside / epiommandol-4’-O-glucoside / Eighteen components, including one unknown compound contained in the 4’-O-glucosidic isomer (2), forsythin, baicalein, taurochenodeoxycholic acid and skullcap extract were all missing , May be the injection of sterile production process using activated carbon adsorption, high temperature sterilization, dosing and other processes and process control using ultrafiltration technology, resulting in differences in the chemical composition of the two preparations. Conclusion: The HPLC-ESIMS / MS analysis method established by this study can effectively characterize the chemical constituents of Tanreqing Capsule and Tanreqing Injection and provide the basis for the quality control of the two preparations.