Ultra-Performance Liquid Chromatography Hyphenated with Quadrupole-Orbitrap Mass Spectrometry for Simultaneous Determination of Necine-Core-Structure Pyrrolizidine Alkaloids in Crotalaria sessiliflora L. without all Corresponding Standards.
BACKGROUND
Crotalaria sessiliflora L. is a Chinese traditional herb for treatment of cutaneum carcinoma and cervical carcinoma. In addition to monocrotaline, coexisting pyrrolizidine alkaloids (PAs) also require further quantification for quality control and pharmaceutical uses of the herb.


OBJECTIVE
To establish a UPLC-Q-Orbitrap/MS method of simultaneous determination of coexisting PAs with same parent structure for quality control and comprehensive researches of Crotalaria sessiliflora L.


METHODS
PAs in Crotalaria sessiliflora L. were analysed by UPLC-Q-Orbitrap/MS method. Coexisting PAs were identified by mass data of full MS-dd-MS2based on the characteristic fragmentation pattern and necine-core structure. Moreover, quantification of PAs was conducted by parallel reaction monitoring (PRM) mode using m/z 138, m/z 120 and m/z 94 from identical necine-core structure as quantitative ions with single monocrotaline standard for accurate calibration.


RESULTS
Five PAs, named monocrotaline, retrorsine, senecionine, integerrimine, O-9-angeloylretronecine, were indentified and confirmed. Quantitative ions of m/z 138, m/z 120 and m/z 94 were used for quantification of PAs containing the necine-core structure in Crotalaria sessiliflora L. The results demonstrated that contents, precision and recoveries of the five PAs mentioned earlier were respectively 3.307-30.35 μg/g, 1.1-4.5% and 88.91-92.33% while using m/z 120 as the best quantitative ion.


CONCLUSIONS
The UPLC-Q-Orbitrap/MS method was established for simultaneous determination of five PAs in Crotalaria sessiliflora L. without all corresponding standards, and was proved that it was simple, convenient and effective for comprehensive quality control and pharmaceutical uses. Copyright © 2017 John Wiley & Sons, Ltd.
School of Basic Course, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Wei
http://orcid.org/0000-0001-5393-4753
W
Zhang
School of Basic Course, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Wenbei
W
Huai
Food Inspection Center, Shenzhen Entry-Exit Inspection and Qurantine Bureau, Shenzhen, Guangdong, 518045, P. R. China.
Yi
Y
Zhang
Food Inspection Center, Shenzhen Entry-Exit Inspection and Qurantine Bureau, Shenzhen, Guangdong, 518045, P. R. China.
Jincan
J
Shen
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Xunyou
X
Tang
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Xiujuan
X
Xie
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Ke
K
Wang
School of Pharmacy, Guangdong Pharmaceutical University, Guangzhou, Guangdong, 510006, P. R. China.
Huajun
H
Fan
D002851:Chromatography, High Pressure Liquid; D029864:Crotalaria / Q000737:chemistry*; D011763:Pyrrolizidine Alkaloids / Q000032:analysis*; D011786:Quality Control; D053719:Tandem Mass Spectrometry
D011763:Pyrrolizidine Alkaloids
Crotalaria sessiliflora L.; Pyrrolizidine alkaloids; UPLC-Q-Orbitrap/MS; monocrotaline; necine-core structure