目的 建立一种全新的基于高效液相色谱与四级杆静电场轨道阱串联质谱联用技术的中药保健品中114种非法添加药物的定性定量筛查方法。方法 以0.1% 甲酸水溶液-乙腈为流动相,采用SHISEIDO CAPCELL PAK C18色谱柱(3.0 mm×100 mm,3 μm),HPLC进行梯度洗脱(0~18 min,乙腈从2%到100%,18~23 min,乙腈为100%,23.1~25 min,乙腈为2%),柱温40 ℃,流速0.3 mL·min-1;质谱采用电喷雾离子源进行扫描,四级杆静电场轨道阱串联质谱作为质量分析器进行采集,扫描范围m/z 120~750,喷雾电压3.5 kV,鞘气压(N2) 275.8 kPa,辅助气压(N2) 68.95 kPa,一次进样即同时获得母离子和碎片子离子的高分辨率高质量精度质谱数据。通过二级质谱精确质量数,对筛查到的非法添加进一步结构确认。结果 本方法在25 min内可同时检测安神类、减肥类、降压类、降脂类、降糖类、抗病毒类、止咳类、止痛类、激素类、精神类、壮阳类共11类114种非法添加化学药物,线性范围、灵敏度、重复性、回收率均满足分析要求。结论 使用高效液相色谱-四级杆静电场轨道阱质谱建立的筛查方法具有快速、便捷、准确的优点,能够满足目标和非目标非法添加的筛查确证需求。
Abstract
OBJECTIVE To establish a new qualitative and quantitative screening method for 114 illegal adulterants in traditional Chinese medicine for health care based on high performance liquid chromatography (HPLC) coupled with high four-stage electrostatic field orbital well tandem mass spectrometry. METHODS Using 0.1% formic acid aqueous solution-acetonitrile as mobile phase, gradient elution was performed on SHISEIDO CAPCELL PAK C18 column(3.0 mm×100 mm,3 μm)with column temperature of 40 ℃ and flow rate of 0.3 mL·min-1. The gradient elution program was as follows: 0-18 min, acetonitrile was from 2% to 100%; 18-23 min, acetonitrile was 100%; 23.1-25 min, acetonitrile was 2%. The mass spectrometry was carried out with electrospray ionization source, four stage electrostatic field track mass spectrometry as mass analyzer, and scanning range m/z 120-750, spray voltage 3.5 kV, sheath pressure (N2) 275.8 kPa, auxiliary air pressure (N2) 68.95 kPa. High resolution and high quality mass spectrometry data of parent ions and fragment ions were obtained simultaneously by one injection. The structures of illegal additions were further confirmed by the accurate mass of secondary mass spectrometry. RESULTS This method could simultaneously detect 114 kinds of illegally added chemical drugs of 11 categories including tranquilizers, hormones, slimming, hypoglycemic, hypotensive, lipid-lowering, psychotropic, antiviral, antitussive, analgesic and aphrodisiac drugs within 25 min. The linear range, sensitivity, repeatability and recovery rate all met the requirements of analysis. CONCLUSION The screening method established by four-stage electrostatic field orbital trap mass spectrometry coupled with HPLC is fast, convenient, accurate and retrospective, and can meet the needs of screening confirmation for target and non-target illegal additions.
关键词
非法添加筛查 /
超高效液相色谱法 /
四级杆静电场轨道阱串联质谱
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Key words
illegal adulterant screening /
liquid chromatograh /
high resolution four-stage electrostatic field mass spectrometry
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中图分类号：
R917
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参考文献
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