超高效液相色谱-三重四级杆质谱法检测阿归养血糖浆中阿胶及牛皮源成分
|
摘要
目的:建立阿归养血糖浆中阿胶及掺杂牛皮源成分的专属性检测方法。方法:用胰蛋白酶对阿归养血糖浆处方中胶类成分进行酶解,采用超高效液相色谱-三重四极杆质谱(UPLC-QQQ/MS),选择阿胶特征分子离子峰m/z 540.0 (双电荷)→612.2、m/z 540.0 (双电荷)→924.4及牛皮源特征离子对m/z 641.3 (双电荷)→726.2、 m/z 641.3 (双电荷)→783.3作为检测离子对,离子化模式为ESI+,进行多反应监测。结果:26批阿归养血糖浆中未检出阿胶的有13批,其中3批检出牛皮源成分,1批检出牛皮源成分但未超出限度,9批均未检出阿胶及牛皮源成分;26批样品检出阿胶的有13批,其中同时检出牛皮源成分的有1批,未检出牛皮源成分的为12批。结论:该检测方法专属性强,可用于阿归养血糖浆中阿胶及牛皮源的检测。
OBJECTIVE To establish an analytical method to identify donkey-hide gelatin and cowhide source in Agui Yangxue syrup. METHODS Identification of donkey-hide gelatin and cowhide source in Agui Yangxue syrup was performed by MRM of rapid resolution liquid chromatography(UPLC) coupled to triple quadruple mass spectrometry(QQQ).RESULTS Thirteen batches of characteristic molecular peaks of donkey-hide gelatin were not detected in the 26 batches of samples, of which 3 batches of cowhide source were detected, and 1 batch was detected but did not exceed the limit, either component was not detected in the 9 batches. Thirteen batches of donkey-hide gelatin were detected in the 26 batches samples, 1 batch of cowhide source was detected, and 12 batches were not detected at the same time. CONCLUSIONMethodological verification shows that the established method is specific, and suitable for the identification of donkey-hide gelatin and cowhide source in Agui Yangxue syrup.
OBJECTIVE To establish an analytical method to identify donkey-hide gelatin and cowhide source in Agui Yangxue syrup. METHODS Identification of donkey-hide gelatin and cowhide source in Agui Yangxue syrup was performed by MRM of rapid resolution liquid chromatography(UPLC) coupled to triple quadruple mass spectrometry(QQQ).RESULTS Thirteen batches of characteristic molecular peaks of donkey-hide gelatin were not detected in the 26 batches of samples, of which 3 batches of cowhide source were detected, and 1 batch was detected but did not exceed the limit, either component was not detected in the 9 batches. Thirteen batches of donkey-hide gelatin were detected in the 26 batches samples, 1 batch of cowhide source was detected, and 12 batches were not detected at the same time. CONCLUSIONMethodological verification shows that the established method is specific, and suitable for the identification of donkey-hide gelatin and cowhide source in Agui Yangxue syrup.
引文
[1] Chinese medicine prescription preparation drag standard of Public Health of China(卫生部药品标准中药成方制剂)[S].Vol12:80.
[2] Ch.P. VolⅠ(中国药典.一部)[S].2015:189.
[3] Ch.P. VolⅠ(中国药典.一部)[S].2015:1228.
[4] National Institutes for Food and Drug Control. Approval of Supplementary test methods and inspection items for Chinese herbal medicine and Chinese herbal medicine[Z].2014013.
[5] National Institutes for Rood and Drug Control. Approval of Supplementary test methods and inspection items for Chinese herbal medicine and Chinese herbal medicine[Z].2011012.
[6] Cheng XL, Chen J, Li MH, et al. Identification Study of Glue Medicine[J]. Journal of Chinese Pharmaceutical Science(中国药学杂志), 2015, 50(2):104-108.
[7] Cheng XL, Wei F, Chen J, et al. Using the doubly charged selected ion coupled with MS/MS fragments monitoring DC SI-MS/MS mode for the identification of gelatin species[J].J Anal Methods Chem, 2014, 764397.
[8] Zhang GF,Liu T, Wang Q, et al. Study of quality control for donkey-hide gelatin[J]. Pharm Bio Technol(药物生物技术),2009, 16(3):250-254.
[9] Cheng XL, Li WJ, Zhang XL, et al. Identification of bovinehide gelatin from glue of tortoise shell and deer-horn gelatin by UPLC-QTOF-MS and principal component analysis[J].Chin J Pharm Anal, 2012,32(6):931-935.
[10] Cheng XL, Wei F, Xiao XY, et al. Identification of five gelatins by ultra performance liquid chromatography/timeof-flight mass spectrometry(UPLC/Q-TOF-MS)using principal component analysis[J].J Pharm Biomed Anal,2012, 62(2):191-195.
[11] Chen J, Cheng XL, Wei F, et al. Qualitative RRLC-QQQ/MS analysis of donkey-hide gelatin in Fufang Ejiao Jiang[J]. Chin J pharm Anal(药物分析杂志),2015, 35(2):328-332.
[12] Chen HY, Li JP, Li WL, et al. Quantitative Detection of donkey-hide gelatin in Fufang Ejiao Buxue Granula by UPLC-QQQ/MS[J]. China Pharmacist(中国药师),2016,19(6):1052-1054.
[13] Long GY, Li MH, Liu W, et al. RRLC/QQQ-MS analysis of donkey-hide gelatin in Ejiao Buxue Granula[J]. Chin J Pharm Anal(药物分析杂志),2016, 36(6):826-829.
[2] Ch.P. VolⅠ(中国药典.一部)[S].2015:189.
[3] Ch.P. VolⅠ(中国药典.一部)[S].2015:1228.
[4] National Institutes for Food and Drug Control. Approval of Supplementary test methods and inspection items for Chinese herbal medicine and Chinese herbal medicine[Z].2014013.
[5] National Institutes for Rood and Drug Control. Approval of Supplementary test methods and inspection items for Chinese herbal medicine and Chinese herbal medicine[Z].2011012.
[6] Cheng XL, Chen J, Li MH, et al. Identification Study of Glue Medicine[J]. Journal of Chinese Pharmaceutical Science(中国药学杂志), 2015, 50(2):104-108.
[7] Cheng XL, Wei F, Chen J, et al. Using the doubly charged selected ion coupled with MS/MS fragments monitoring DC SI-MS/MS mode for the identification of gelatin species[J].J Anal Methods Chem, 2014, 764397.
[8] Zhang GF,Liu T, Wang Q, et al. Study of quality control for donkey-hide gelatin[J]. Pharm Bio Technol(药物生物技术),2009, 16(3):250-254.
[9] Cheng XL, Li WJ, Zhang XL, et al. Identification of bovinehide gelatin from glue of tortoise shell and deer-horn gelatin by UPLC-QTOF-MS and principal component analysis[J].Chin J Pharm Anal, 2012,32(6):931-935.
[10] Cheng XL, Wei F, Xiao XY, et al. Identification of five gelatins by ultra performance liquid chromatography/timeof-flight mass spectrometry(UPLC/Q-TOF-MS)using principal component analysis[J].J Pharm Biomed Anal,2012, 62(2):191-195.
[11] Chen J, Cheng XL, Wei F, et al. Qualitative RRLC-QQQ/MS analysis of donkey-hide gelatin in Fufang Ejiao Jiang[J]. Chin J pharm Anal(药物分析杂志),2015, 35(2):328-332.
[12] Chen HY, Li JP, Li WL, et al. Quantitative Detection of donkey-hide gelatin in Fufang Ejiao Buxue Granula by UPLC-QQQ/MS[J]. China Pharmacist(中国药师),2016,19(6):1052-1054.
[13] Long GY, Li MH, Liu W, et al. RRLC/QQQ-MS analysis of donkey-hide gelatin in Ejiao Buxue Granula[J]. Chin J Pharm Anal(药物分析杂志),2016, 36(6):826-829.