Determination of Paclobutrazol Residue in Ophiopogon japonicus from Sichuan by the QuEChERS Combined with GC-MS/ MS-internal Standard Detection
- VernacularTitle:QuEChERS结合GC-MS/MS-内标法测定川麦冬中多效唑残留量
- Author:
Yan GOU
1
,
2
;
Chi GAO
1
;
Jingjing DENG
1
;
Hongyan LI
1
;
Zhao GENG
1
,
2
;
Juan ZHOU
2
;
Jun YUAN
2
;
Min LI
1
Author Information
1. College of Pharmacy，Chengdu University of TCM，Chengdu 611137，China
2. Sichuan Provincial Institute for Food and Drug Control，Chengdu 611731，China
- Publication Type:Journal Article
- Keywords:
Ophiopogon japonicus from Sichuan;
GC-MS/MS;
Internal standard;
Paclobutrazol;
Residue
- From:
China Pharmacy
2019;30(3):323-327
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE： To establish a method for measuring the paclobutrazol residue in Ophiopogon japonicus from Sichuan and detect the quality of O. japonicus from Sichuan from different sources. METHODS： Totally 50 batches of samples were collected from different origin places， commercial markets and manufacturers. The sample pretreatment method was QuEChERS method， .ie the sample was extracted by aqueous acetonitrile， salted out by QuEChERS extract package （containing anhydrous magnesium sulfate and anhydrous sodium acetate）， the extract solution was purified by QuEChERS purification package （containing anhydrous magnesium sulfate， N-propyl ethylenediamine， octadecylsilane chemically bonded silica， silica gel， graphitized carbon black） and then added into internal standard triphenyl phosphate. The paclobutrazol residue in O. japonicus from Sichuan was determined by GC-MS/MS. The determination was performed on DB-5MS column. The temperature programming was adopted， and the detector was triple quadrupole MS detector. The initial flow rate of carrier gas was 1.3 mL/min； acquisition mode was MRM. Injection method was splitless injection. RESULTS： The linear range of paclobutrazol was 1.01-505 ng/mL （r＝ 0.999 7）. RSDs of precision， stability （24 h） and repeatability tests were 3.94％， 13.62％， 7.54％ （n＝6）， respectively. Average method recovery was 111.26％ （RSD＝5.43％， n＝9）. The paclobutrazol residue in 50 batches of sample were 0.02-2.72 mg/kg. CONCLUSIONS： Established method is simple， accurate， sensitive and reproducible. It also can be used for the determination of paclobutrazol residue in O. japonicus from Sichuan. The contents of paclobutrazol residue in O. japonicus from Sichuan from different sources are different greatly.
