Determination of Donkey-hide Gelatin in Lüjiao Buxue Granules by UPLC-QQQ/MS
10.6039/j.issn.1001-0408.2017.15.24
- VernacularTitle:UPLC-QQQ/MS法检测驴胶补血颗粒中的阿胶
- Author:
Hongyu CHEN
;
Jinping LI
;
Wenli LI
;
Ye DING
;
Hui SUN
;
Qing YANG
;
Xiaoyan HUANG
- Keywords:
UPLC-QQQ/MS;
Lüjiao buxue granules;
Donkey-hide gelatin;
Characteristic molecular ion peak
- From:
China Pharmacy
2017;28(15):2101-2104
- CountryChina
- Language:Chinese
-
Abstract:
OBJECTIVE:To establish a method for the determination of donkey-hide gelatin in Lüjiao buxue granules. METH-ODS:Trypsin was used for enzymatic hydrolysis of donkey-hide gelatin. UPLC-QQQ/MS was adopted for the determination of don-key-hide gelatin in the preparation:Hypersil GOLD C18 column was used with mobile phase consisted of 0.1% formic acid solu-tion-acetonitrile(gradient elution)at the flow rate of 0.3 mL/min. The column temperature was 30 ℃,and sample size was 5 μL. Mass chromatography condition was that ion source was electrospray ion source;ionization mode was ESI+;multiple response mon-itoring was adopted,and characteristic molecular ion peaks of donkey-hide gelatin with mass-to-charge ratio of m/z 539.8(double charge)→ 612.4 and m/z 539.8(double charge)→ 923.8 were used as detection ion pair. Spray voltage was 3100 V;sheath gas was 20 Arb;auxiliary gas was 8 Arb;ion transfer tube temperature was 350 ℃;evaporation temperature was 350 ℃;scan mode was SRM. Collision gas was high purity argon. RESULTS:The sample size of donkey-hide gelatin ranged 20.24-2024 μg/mL(r=0.9978). The detection limit was 1%. RSDs of precision,stability and reproducibility tests were all lower than 6.0%. The charac-teristic molecular ion peaks of donkey-hide gelatin could be detected in 27 batches of samples. CONCLUSIONS:The method is spe-cific and can be used for the determination of donkey-hide gelatin in Lüjiao buxue granules.
