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刊物信息

期刊名称:药物分析杂志
主管单位:中国科学技术协会
主办单位:中国药学会
承办:中国食品药品检定研究院
主编:金少鸿
地址:北京天坛西里2号
邮政编码:100050
电话:010-67012819,67058427
电子邮箱:ywfx@nicpbp.org.cn
国际标准刊号:ISSN 0254-1793
国内统一刊号:CN 11-2224/R
邮发代号:2-237
 

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超高效液相色谱-三重四极杆质谱法用于阿胶、龟甲胶、鹿角胶中猪皮源成分的检测

Detection of pig-hide gelatin adulteration in deer-horn glue,tortoise-shell glue and donkey-hide gelatin by UPLC-QQQ/MS

分类号:R917
出版年·卷·期(页码):2020,40 (5):859-864
DOI: 10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------

目的:建立超高效液相色谱-三重四极杆质谱法(UPLC-QQQ/MS法)测定阿胶、龟甲胶和鹿角胶中猪皮源成分。方法:采用胰蛋白酶进行酶解处理,色谱柱为ZORBAX SB-C18(2.1 mm×150 mm,5 μm);以0.1%甲酸溶液(A)-乙腈(B)为流动相,梯度洗脱(0~25 min,95%A→80%A;25~40 min,80%A→50%A),流速为0.3 mL·min-1;电喷雾离子源(ESI),正离子模式下扫描,采用多重反应监测模式(MRM),对特征肽目标离子m/z 774.5(双电荷)→977.8和m/z 774.5(双电荷)→1 034.6进行检测。结果:阿胶中新阿胶掺入量为1%~12%、龟甲胶中新阿胶掺入量为2%~11%、鹿角胶中新阿胶掺入量为3%~12%的范围内,掺入量与色谱峰面积成正比,线性方程分别为Y=4 471X-29.00(r2=0.997 1),Y=4 468X-63.33(r2=0.996 3),Y=4 262X-74.48(r2=0.998 0)。检测下限浓度为0.1 g·mL-1。5批阿胶、5批龟甲胶、5批鹿角胶中,有1批阿胶、1批龟甲胶、2批鹿角胶可疑样品中检出新阿胶。结论:所建立方法操作简便,专属性强,灵敏度高,重复性良好,可用于阿胶、龟甲胶和鹿角胶中掺伪成分猪皮源的检测。

-----英文摘要:---------------------------------------------------------------------------------------

Objective: To establish a ultra-high performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-QQQ/MS) method for the identification of ingredients from pig skin in donkey-hide gelatin,tortoise-shell glue and deer-horn glue. Methods: Trypsin was used for enzymatic hydrolysis. UPLC-QQQ/MS was used to detect ingredients from pig skin in donkey-hide gelatins,tortoise-shell glue and deer-horn glue. Determination was carried out by means of an Agilent SB-C18(2.1 mm×150 mm,1.8 μm) column. The mobile phase was composed of water solvent containing 0.1% formic acid(A)and acetonitrile(B)with gradient elution(0-25 min,95%A→80%A;25-40 min,80%A→50%A)at the flow rate of 0.3 mL·min-1. The electrospray ionization(ESI)source was performed in multiple reaction monitoring(MRM)mode of the transitions of m/z 774.5(double-charge)→977.8 and m/z 774.5(double-charge)→1 034.6. Results: The adulteration rate was proportional to the chromatographic peak area when the adulteration pig-hide gelatin was 1%-12% in donkey-hide gelatin,2%-11% in tortoise-shell glue and 3%-12% in deer-horn glue,respectively. The linear equations were Y=4 471X-29.00(R2=0.997 1),Y=4 468X-63.33(R2=0.996 3),and Y=4 262X-74.48(R2=0.998 0),respectively. The lower limit of detection concentration of pig-hide gelatin was 0.1 g·mL-1. Ingredients from pig skin can be detected in one of fives batches of donkey-hide gelatin,one of fives batches of tortoise-hide gelatin and two of fives batches of deer-horn gelatin. Conclusion: The established method is simple,specific,sensitive and repetitive. It can be used for identification of ingredients from pig skin in donkey-hide gelatin,tortoise-shell glue and deer-horn glue.

-----参考文献:---------------------------------------------------------------------------------------
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