[1]张生杰,王丽,曹雪芹,等.高效液相色谱-质谱法测定宣肺止嗽合剂中吗啡含量[J].甘肃中医药大学学报,2020,37(01):47-52.[doi:10.16446/j.cnki.1001-1994.2020.01.010]
 ZHANG Shengjie,WANG Li,CAO Xueqin,et al.Content determination of morphinum in Xuanfei Zhisou Heji(宣肺止嗽合剂) by HPLC-MS[J].Journal of Gansu University of Chinese Medicine,2020,37(01):47-52.[doi:10.16446/j.cnki.1001-1994.2020.01.010]
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高效液相色谱-质谱法测定宣肺止嗽合剂中吗啡含量
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《甘肃中医药大学学报》[ISSN:1003-8450/CN:62-1062/R]

卷:
37卷
期数:
2020年01期
页码:
47-52
栏目:
技术与方法
出版日期:
2020-02-25

文章信息/Info

Title:
Content determination of morphinum in Xuanfei Zhisou Heji(宣肺止嗽合剂) by HPLC-MS
作者:
张生杰 王丽 曹雪芹 田志梅
武威市药品检验检测中心中药检验科, 甘肃 武威 733000
Author(s):
ZHANG Shengjie WANG Li CAO Xueqin TIAN Zhimei
Laboratory of Chinese Materia Medica, Wuwei Institute for Drug Control, Wuwei, Gansu, 733000, China
关键词:
宣肺止嗽合剂吗啡高效液相色谱-质谱含量测定
Keywords:
Xuanfei Zhisou Heji(宣肺止嗽合剂)morphinumHPLC-MScontent determination
分类号:
R284.1
DOI:
10.16446/j.cnki.1001-1994.2020.01.010
摘要:
目的 建立高效液相色谱-质谱(HPLC-MS)法测定宣肺止嗽合剂中吗啡含量的方法。方法 采用HPLC-MS正离子多反应监测模式(MRM)测定宣肺止嗽合剂中吗啡的含量,色谱柱为Shim-pack GIST-HP C18柱(50.0 mm×2.1 mm,3 μm),流动相为甲醇-0.1%甲酸(30∶70,V/V),流速0.3 mL/min,柱温40 ℃;采用电喷雾离子源(ESI),以MRM进行定量分析,吗啡在正离子模式下定量分析离子对m/z 286.40→m/z 201.10。结果 吗啡在0.517 5~5.175 0 μg/mL质量浓度范围内线性关系良好(r=0.999 3);平均加样回收率为98.34%,RSD为1.44%;最低检测限为0.207 ng/mL,最低定量限为0.414 ng/mL。结论 该方法简单可靠、重复性好,适用于药品中低含量吗啡的检测。
Abstract:
Objective To establish a high performance liquid chromatography-mass spectrometry(HPLC-MS) method for content determination of morphinum in Xuanfei Zhisou Heji(宣肺止嗽合剂). Methods The morphine content was determined by HPLC-MS positive ion multiple reaction monitoring mode(MRM).The chromatographic column used was Shim-pack GIST-HP C18 (50.0 mm×2.1 mm,3 μm). The mobile phase was a solution comprising methanol and 0.1% formic acid (30∶70,V/V). The flow rate was 0.3 mL/min,and the column temperature was 40 ℃. Using electrospray ionization(ESI) source,the quantative analysis was performed with multiple reactions monitoring mode(MRM). The quantitative analysis of morphine in the positive ion mode showed that the ion pair was m/z 286.40→m/z 201.10. Results Good linearity was obtained with morphinum concentration ranging from 0.517 5 to 5.175 0 μg/mL(r=0.999 3) with the average recovery of 98.34%,RSD 1.44%,the minimum detection limit 0.207 ng/mL and the limit of quantification(LOQ) 0.414 ng/mL. Conclusion The method is simple,reliable and reproducible,which is suitable for content determination of low content morphine in medicinal.

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备注/Memo

备注/Memo:
收稿日期:2019-01-04。
作者简介:张生杰(1985-),男,主管中药师,医学硕士,主要从事中药鉴定及质量标准研究。
更新日期/Last Update: 1900-01-01