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纸质出版日期:2013
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樊磊磊, 刘乃强, 李振国. UPLC-MS定性定量检测稳糖安胶囊中降糖类化学药品[J]. 中国实验方剂学杂志, 2013,19(8):87-91.
FAN Lei-lei, LIU Nai-qiang, LI Zhen-guo. Qualitative and Quantitative Determination of Antidiabetic Drugs in Wentangan Capsule by UPLC-MS[J]. Chinese journal of experimental traditional medical formulae, 2013, 19(8): 87-91.
樊磊磊, 刘乃强, 李振国. UPLC-MS定性定量检测稳糖安胶囊中降糖类化学药品[J]. 中国实验方剂学杂志, 2013,19(8):87-91. DOI: 10.11653/syfj2013080087.
FAN Lei-lei, LIU Nai-qiang, LI Zhen-guo. Qualitative and Quantitative Determination of Antidiabetic Drugs in Wentangan Capsule by UPLC-MS[J]. Chinese journal of experimental traditional medical formulae, 2013, 19(8): 87-91. DOI: 10.11653/syfj2013080087.
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
3 μm)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 an UPLC-MS method for determination of antidiabetic drugs in Wentangan capsule. Method: Ultra performance liquid chromatography tandem quadrupole mass spectrometer was adopted
LC condition: A agela Venusil-C18 (2.1 mm×50 mm
3 μm) column was used with the isocratic elution of acetonitrile and 0.01 mol·L-1 ammonium acetate at a flow rate of 0.2 mL·min-1. MS condition: adopted electrospray ionization (ESI)
and multiple reaction monitoring (MRM); monitoring by ion-pairs: 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)
phenethylbiguanide (206.2→59.7
206.2→104.6)
dimethyl biguanide (130.1→60.0
130.1→71.0). The retention time and relative intensities of the detected qualitative ion pairs using for qualitative
integrating the signals of the detected quantitative ion pairs using for quantitative. Result: The eight kinds of antidiabetic drugs had good linearity with correlation coefficient>0.999
ranging from 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 and 4.264
136.448 ng·L-1 respectively. The average recoveries were 98.18-100.95%. Repeatability experiments showed that RSD values of content were less than 2.95%. Conclusion: This method is reliable
simple and rapid with qualitative and quantitative accuracy
can be used for determination of antidiabetic drugs illegally added in Wentangan capsule.
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