
高效液相色谱-串联质谱法快速筛查药用复合包装袋中8种水溶性杂质
余秋玲, 张云冉, 邱月, 龙梅, 杨倩, 陆嘉莉
高效液相色谱-串联质谱法快速筛查药用复合包装袋中8种水溶性杂质
Rapid Screening of eight Water-soluble Impurities in Medicinal Composite Packaging Bag by HPLC-MS/MS Method
建立了同时测定药用复合包装袋中8种水溶性杂质的高效液相色谱-串联质谱法(HPLC-MS/MS)。将药用复合包装袋剪碎,采用超纯水在50 ℃条件下超声提取30 min。提取液经0.22 μm聚四氟乙烯(PTFE)微孔滤膜过滤后,以甲醇-0.1%甲酸为流动相进行梯度洗脱,经ZORBAX Eclipse XDB-C18(3.5 μm,4.6 mm×150.0 mm)色谱柱分离,在ESI源正离子模式下进行多反应监测(MRM)扫描,采用外标法定量。对色谱柱、流动相和质谱参数进行优化,并对基质效应进行评价。结果表明:最优条件下的检出限(LOD)为0.20~0.35 ng/g,线性相关系数均高于0.995,平均加标回收率为85.0%~115.8%,相对标准偏差(RSD)为0.3%~9.2%(n=6)。该方法前处理简单,分析时间短至6 min,无明显基质效应,可用于药用复合包装袋中8种水溶性杂质的快速筛查。
A method for determining eight water-soluble impurities in medicinal composite packaging bag by HPLC-MS/MS simultaneously was established. The medicinal composite packaging bag was cut into small pieces and then extracted by ultrapure water with ultrasonic wave at 50 ℃ for 30 min, followed by clean-up through a 0.22 μm polytetrafluoroethylene (PTFE) membrane. The separation was conducted on ZORBAX Eclipse XDB-C18 (3.5 μm, 4.6 mm×150.0 mm) with methanol-0.1% formic acid as mobile phase. The target compounds were detected under electrospray ionization (ESI) positive ion multiple reactive monitoring (MRM) mode, and quantified by external standard method. The chromatographic column, mobile phase and mass spectrum parameters were optimized, and the matrix effect was assessed. The results showed that the limits of determination (LOD) were 0.20~0.35 ng/g, the linear correlation coefficients were all higher than 0.995, the average recoveries were 85.0%~115.8%, and the RSD were 0.3%~9.2% (n=6) under the optimized conditions. The method exhibited the advantages of simple pretreatment, short analysis time (6 min) and slight matrix effect, which can be used for the rapid screening of eight water-soluble impurities in medicinal composite packaging bag.
水溶性杂质 / 高效液相色谱-串联质谱法 / 药用复合包装袋
Water-soluble impurity / HPLC-MS/MS / Medicinal composite packaging bag
O657.63
1 |
汪世宁,崔江水,罗弘宇,等.印刷行业典型挥发性有机物的排放特征与管控措施综述[J].环境工程,2023,41():306-313, 319.
增刊1
|
2 |
梁小明,吴彭珍,陈来国,等.中国印刷业VOCs排放趋势及未来减排潜力[J].环境科学,2023,44(11):5915-5923.
|
3 |
国家药品监督管理局. 双向拉伸聚丙烯/真空镀铝流延聚丙烯药用复合膜、袋:YBB00192004—2015 [S].北京:中国医药科技出版社,2015.
|
4 |
苏毅,张军.口服固体制剂包装中药用铝箔及药用复合膜的质量控制[J].印刷技术,2021(1):40-42.
|
5 |
邓孙艳,李鋆,黄毅萍,等.HTPB改性UV固化水性聚氨酯油墨的合成[J].塑料,2022,51(4):66-70, 75.
|
6 |
钱凯,李伟涛,葛文秀,等.超高效液相色谱-串联质谱法测定纸制食品接触材料中丙烯酰胺的迁移量[J].分析测试学报,2021,40(11):1645-1650.
|
7 |
黄海智,盛华栋,李红艳,等.包装纸中丙烯酰胺及芳香胺迁移量的检测研究[J].包装工程,2018,39(13):27-31.
|
8 |
European Chemicals Agency. N,N-dimethylacrylamide[EB/OL]. [2023-07-07].
|
9 |
European Chemicals Agency. N-(hydroxymethyl)acrylamide[EB/OL]. [2023-07-07].
|
10 |
张清,邱月,余秋玲,等.GC-MS法测定药用复合包装袋中异氰酸酯[J].包装工程,2021,42(9):177-183.
|
11 |
李家春,孙兰,翁晓滨,等.聚氨酯输液器中7种异氰酸酯成分的提取与2种抗氧剂的溶出研究[J].塑料科技,2023,51(10):96-101.
|
12 |
钟艳琴,张静,胡洁兰,等.毛细管电泳法测定食品塑料包装材料中2,4-二氨基甲苯[J].分析试验室,2014,33(6):729-732.
|
13 |
李静,张居舟,刘毅,等.UPLC-MS/MS法测定包装材料中5种二氨基甲苯的迁移量[J].食品工业,2021,42(6):472-476.
|
14 |
European Chemicals Agency. Benzyldimethylamine[EB/OL]. [2023-07-07].
|
15 |
高松,王志伟,胡长鹰,等.食品包装油墨迁移研究进展[J].食品科学,2012,33(11):317-322.
|
16 |
余德金.塑料凹印中的色迁移和色渗透[J].印刷杂志,2005(8):68-69.
|
17 |
饶艳春,熊马剑,汪元亮,等.高效液相色谱法测定聚氯乙烯固体药用硬片中17种添加剂[J].塑料科技,2023,51(6):53-58.
|
18 |
余秋玲,张清,陆嘉莉,等.无衍生化-气相色谱-质谱联用法测定药用溴化丁基胶塞中硬脂酸和软脂酸的可提取量和迁移量[J].分析试验室,2021,40(4):469-473.
|
19 |
杜芹芹.HS-GC-MS法测定药用复合膜中15种溶剂残留量[J].塑料科技,2022,50(5):93-97.
|
20 |
梅丽芳,刘盈君,谢新艺.常用药用复合材料中的2,4-二氨基甲苯含量对比探讨[J].塑料包装,2019,29(6):41-45.
|
21 |
罗佳,吴春霞,周晓龙.同位素内标超高效液相色谱-串联质谱法测定膨化食品中丙烯酰胺[J].中国卫生检验杂志,2022,32(14):1695-1698.
|
22 |
郇志博,段云,徐志,等.超高压液相色谱-串联质谱法测定速溶咖啡和曲奇饼干中丙烯酰胺的含量[J].理化检验:化学分册,2021,57(10):913-918.
|
23 |
李莎,武静文,吴红洋,等.药用复合膜中2,4-二氨基甲苯的检测[J].药物分析杂志,2022,42(7):1234-1240.
|
24 |
郭娟娟,唐熙,陈丽娟,等.超声提取-气相色谱-质谱法同时测定尼龙等食品接触材料中5种酰胺类物质[J].理化检验:化学分册,2020,56(6):696-700.
|
25 |
茅文良,卢坤,于立莹,等.柱前衍生GC-MS法测定纺织品中丙烯酰胺和甲基丙烯酰胺[J].印染,2022,48(6):71-74.
|
26 |
邹茄,朱碧君,常亮,等.GC-MS法测定药用复合膜中25种初级芳香胺的迁移量[J].中国新药杂志,2021,30(7):649-653.
|
27 |
刘海霞,狄婧,饶红红,等.纳米二氧化锰固相萃取-高效液相色谱法测定油炸食品中丙烯酰胺[J].理化检验:化学分册,2019,55(12):1373-1378.
|
28 |
邵美丽,郝星宇,刘巍,等.固相萃取-高效液相色谱法检测油炸猪肉中丙烯酰胺[J].食品科学,2015,36(8):231-235.
|
29 |
林型跑,陈海相,孙岩峰,等.高效液相色谱法测定纺织品中丙烯酰胺、甲基丙烯酰胺和N-羟甲基丙烯酰胺[J].现代纺织技术,2019,27(1):80-86.
|
30 |
唐会鑫,谷悦,郭二菱,等.超高效液相色谱-串联质谱法同时测定土壤中13种硝基咪唑类抗生素的含量[J].理化检验-化学分册,2023,59(5):606-611.
|
31 |
王园媛,李璐璐,吕佳,等.固相萃取-超高效液相色谱-三重四极杆质谱法测定饮用水中13种卤代苯醌类消毒副产物[J].色谱,2023,41(6):482-489.
|
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|
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