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目的:建立UPLC-MS方法,快速定性定量检测稳糖安胶囊中非法添加的降糖类化学药品。方法:采用超高效液相色谱串联四极杆质谱仪,色谱条件:Agela Venusil-C18(2.1 mm×50 mm,3μm)色谱柱,柱温35℃,流动相乙腈-0.01 mol·L-1乙酸铵(50∶50),流速0.2 mL·min-1。质谱条件:ESI源,多反应检测(MRM),监测离子对(m/z):瑞格列奈(453.4→86.0,453.4→230.3)、格列美脲(491.4→126.2,491.4→352.3)、格列本脲(494.2→168.5,494.2→368.9)、吡格列酮(357.2→119.0,357.2→134.1)、格列齐特(342.2→90.9,324.2→109.9)、格列吡嗪(446.2→92.6,446.2→102.6)、苯乙双胍(206.2→59.7,206.2→104.6)、二甲双胍(130.1→60.0,130.1→71.0)。以保留时间和定性离子对之间的相对丰度定性,以定量离子对峰面积定量。结果:8种降糖化学药品瑞格列奈、格列美脲、格列本脲、盐酸吡格列酮、格列齐特、格列吡嗪、盐酸苯乙双胍、盐酸二甲双胍分别在4.056～129.792,13.912～125.184,3.92～125.44,3.944～126.208,4.056～129.792,4.232～135.424,4.072～130.304,4.264～136.448 ng·L-1均呈现良好的线性关系(r>0.999);平均加样回收率均在98.18～100.95%;8种降糖化学药品含量重复性试验RSD<2.95%。结论:方法定性可靠、定量准确,且快速简便,可用于稳糖安胶囊中非法添加的降糖类化学药品检测。
OBJECTIVE: To establish a UPLC-MS method to rapidly and qualitatively and quantitatively detect the hypoglycemic chemicals illegally added in Wentangan capsules. Methods: The chromatographic conditions were: Agela Venusil-C18 column (2.1 mm × 50 mm, 3 μm), column temperature 35 ℃, mobile phase acetonitrile-0.01 mol·L-1 acetic acid Ammonium (50:50), flow rate 0.2 mL · min-1. Mass spectrometry conditions: ESI source, multiple reaction detection (MRM), monitored ion pair (m / z): repaglinide (453.4 → 86.0,453.4 → 230.3), glimepiride (491.4 → 126.2, 491.4 → 352.3) Glibenclamide (494.2 → 168.5, 494.2 → 368.9), pioglitazone (357.2 → 119.0, 357.2 → 134.1), gliclazide (342.2 → 90.9, 324.2 → 109.9), glipizide (446.2 → 92.6, 446.2 → 102.6), phenformin (206.2 → 59.7, 206.2 → 104.6), metformin (130.1 → 60.0, 130.1 → 71.0). The relative abundance between the retention time and the qualitative ion pair was qualitatively quantified by quantitation of the ion peak area. Results: 8 kinds of anti-diabetic drugs repaglinide, glimepiride, glibenclamide, pioglitazone hydrochloride, gliclazide, glipizide, phenformin hydrochloride, metformin hydrochloride were 4.056 ~ 129.792, 13.912 ~ 125.184,3.92 ~ 125.44,3.944 ~ 126.208,4.056 ~ 129.792,4.232 ~ 135.424,4.072 ~ 130.304,4.264 ~ 136.448 ng · L-1 all showed a good linear relationship (r> 0.999) 98.18 ~ 100.95%. The RSDs of 8 kinds of hypoglycemic chemicals were less than 2.95%. Conclusion: The method is qualitative and reliable, quantitative and accurate, and fast and easy. It can be used to detect the hypoglycemic chemicals illegally added in Wentangan capsules.