玄麦甘桔制剂中多效唑残留量检测  

Detection of Paclobutrazol Residues in Xuanmai Ganju Preparation

作　　者：胡亮 孙辉 丁野 罗艳 李文莉 李靖云 HU Liang;SUN Hui;DING Ye;LUO Yan;LI Wenli;LI Jingyun(Hunan Institute for Drug Control,Changsha,Hunan,China 410001;Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha,Hunan,China 410001)

机构地区：[1]湖南省药品检验检测研究院,湖南长沙410001 [2]湖南省药品质量评价工程技术研究中心,湖南长沙410001

出　　处：《中国药业》2023年第20期94-97,共4页China Pharmaceuticals

基　　金：2022年国家药品抽验专项。

摘　　要：目的建立检测玄麦甘桔制剂中多效唑残留量的超高效液相色谱串联质谱(UPLC-MS/MS)法。方法色谱柱为WelchUltimate LP-C_(18)柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-含0.1%甲酸的5 mmol/L乙酸铵溶液(55∶45,V/V),流速为0.2 mL/min,柱温为30℃,进样量为3μL;采用电喷雾离子源正离子(ESI+),多反应监测(MRM)模式,检测离子对为m/z 294.0→70.2、m/z 294.0→125.0。结果多效唑质量浓度在4.812~240.6 ng/mL范围内与离子相对丰度线性关系良好(r=0.9998);仪器检测限为0.11 pg,方法检测限为0.055 ng/g(含糖型颗粒剂、胶囊剂、片剂),0.11 ng/g(无糖型颗粒剂)。精密度、稳定性、重复性试验结果的RSD均小于3.0%;平均加样回收率为86.87%,RSD为3.33%(n=6)。237批次样品中有208批次(87.76%)检出多效唑,3种剂型(颗粒剂、胶囊剂、片剂)均有涉及,最高残留量为0.3773 mg/kg;24批次超出拟订限度,均为含糖型颗粒剂。结论该方法操作简便、结果准确,可用于检测玄麦甘桔制剂中多效唑的残留量。Objective To establish an ultra-high-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)method for the detection of paclobutrazol residues in Xuanmai Ganju Preparation.Methods The chromatographic column was Welch Ultimate LP-C_(18)column(100 mm×2.1 mm,1.8μm),the mobile phase was acetonitrile-5 mmol/L ammonium acetate solution containing 0.1%formic acid(55∶45,V/V),the flow rate was 0.2 mL/min,the column temperature was 30℃,and the injection volume was 3μL.The positive-ion electro-spray ionization(ESI+)was adopted with the multiple reaction monitoring(MRM)mode,the detected ion pair was m/z 294.0→70.2,m/z 294.0→125.0.Results The linear range of paclobutrazol was 4.812-240.6 ng/mL(r=0.9998).The limit of detection of instrument was 0.11 pg,the limits of detection of method were 0.055 ng/g(sugar-containing granules,capsules,tablets)and 0.11 ng/g(sugar-free granules).The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rate of paclobutrazol was 86.87%with an RSD of 3.33%(n=6).Among the 237 batches of samples,paclobutrazol was detected in 208 batches(87.76%),involving three dosage forms(granules,capsules and tablets),with a maximum residues of 0.3773 mg/kg.Paclobutrazol in 24 batches of samples was over the prescribed limit,and these samples were all sugar-containing granules.Conclusion This method is simple and accurate,which can be used to detect the residues of paclobutrazol in Xuanmai Ganju Preparation.

关 键 词：超高效液相色谱串联质谱法 玄麦甘桔制剂 多效唑 

分 类 号：R917[医药卫生—药物分析学] R927[医药卫生—药学]