浙江中医药大学学报
浙江中醫藥大學學報
절강중의약대학학보
JOURNAL OF ZHEJIANG UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
2015年
8期
615-620
,共6页
快速高分离液相色谱-质谱法%减肥药%盐酸西布曲明%呋塞米%盐酸麻黄碱%含量
快速高分離液相色譜-質譜法%減肥藥%鹽痠西佈麯明%呋塞米%鹽痠痳黃堿%含量
쾌속고분리액상색보-질보법%감비약%염산서포곡명%부새미%염산마황감%함량
RRLC-MS%diet pills%sibutramine hydrochloride%furosemide%ephedrine hydrochloride%content
[目的]建立盐酸西布曲明、呋塞米和盐酸麻黄碱的快速高分离液相色谱-质谱联用(rapid resolution liquid chromatography-mass spectrometry, RRLC-MS)方法,检测7种减肥药中是否含有非法添加成分。[方法]色谱条件:Agilent SB-C18柱(2.1mm×50mm,5μm),乙腈(含0.1%甲酸)-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.2mL·min-1;质谱条件:电喷雾离子(electrospray ionization, ESI)源,以正负离子、多反应监测(multiple reaction monitoring, MRM)扫描模式检测减肥药中违禁成分。[结果]7种减肥药中均检测到盐酸西布曲明和盐酸麻黄碱,含量范围分别为0.39~4.29μg·g-1和1.63~8984.18μg·g-1,1种减肥药中检测到呋塞米,含量为8.71μg·g-1。[结论]本研究建立的快速高分离液相色谱-质谱联用法方便快捷、灵敏度好、准确度高,适用于减肥药中非法添加成分的定性定量检测。
[目的]建立鹽痠西佈麯明、呋塞米和鹽痠痳黃堿的快速高分離液相色譜-質譜聯用(rapid resolution liquid chromatography-mass spectrometry, RRLC-MS)方法,檢測7種減肥藥中是否含有非法添加成分。[方法]色譜條件:Agilent SB-C18柱(2.1mm×50mm,5μm),乙腈(含0.1%甲痠)-0.1%甲痠水溶液為流動相進行梯度洗脫,流速0.2mL·min-1;質譜條件:電噴霧離子(electrospray ionization, ESI)源,以正負離子、多反應鑑測(multiple reaction monitoring, MRM)掃描模式檢測減肥藥中違禁成分。[結果]7種減肥藥中均檢測到鹽痠西佈麯明和鹽痠痳黃堿,含量範圍分彆為0.39~4.29μg·g-1和1.63~8984.18μg·g-1,1種減肥藥中檢測到呋塞米,含量為8.71μg·g-1。[結論]本研究建立的快速高分離液相色譜-質譜聯用法方便快捷、靈敏度好、準確度高,適用于減肥藥中非法添加成分的定性定量檢測。
[목적]건립염산서포곡명、부새미화염산마황감적쾌속고분리액상색보-질보련용(rapid resolution liquid chromatography-mass spectrometry, RRLC-MS)방법,검측7충감비약중시부함유비법첨가성분。[방법]색보조건:Agilent SB-C18주(2.1mm×50mm,5μm),을정(함0.1%갑산)-0.1%갑산수용액위류동상진행제도세탈,류속0.2mL·min-1;질보조건:전분무리자(electrospray ionization, ESI)원,이정부리자、다반응감측(multiple reaction monitoring, MRM)소묘모식검측감비약중위금성분。[결과]7충감비약중균검측도염산서포곡명화염산마황감,함량범위분별위0.39~4.29μg·g-1화1.63~8984.18μg·g-1,1충감비약중검측도부새미,함량위8.71μg·g-1。[결론]본연구건립적쾌속고분리액상색보-질보련용법방편쾌첩、령민도호、준학도고,괄용우감비약중비법첨가성분적정성정량검측。
Objective]To establish a rapid resolution liquid chromatography-mass spectrometry(RRLC-MS) method for sibutramine hydrochloride, ephedrine hydrochloride and furosemide, which is the illegally added substances in diet pills. [Method]The chromatographic conditions: Agilent SB-C18 column(2.1mm×50mm, 5μm). The mobile phase consists of acetonitrile(containing 0.1% formic acid) and 0.1% formic acid solution, gradient elution with flow rate of 0.2mL·min-1; The MS conditions: electrospray ionization(ESI) source, with positive and negative ions, multiple reaction monitoring(MRM) mode to detect contents of prohibited substances in diet pills. [Result]Under the above conditions, all seven diet pills were detected with the sibutramine hydrochloride and ephedrine hydrochloride. The concentration range of the two substances was from 0.39 to 4.29μg·g-1 and from 1.63 to 8984.18μg·g-1 respectively. One drug contained furosemide, while the content was 8.71μg·g-1. [Conclusion]The method established was fast, convenient, had high sensitivity and high accuracy, which can detect prohibited substances quantitatively and qualitatively in diet pills.