摘要
目的测定药用复合膜中苯二胺含量,并制定限度标准。方法采用岛津Rtx-5毛细管色谱柱(30 m×0.25 mm,0.25μm),温度进样口为200℃、气化室为220℃、FID为300℃,载气高纯度氮气流速为0.8 m L/min,氢气流速为40 m L/min,空气流速为400 m L/min,尾吹流速为30 m L/min,柱温为程序升温(初始温度为100℃,保持1 min,以20℃/min的速率升至200℃,保持0 min,再以20℃/min的速率升至280℃,保持10 min),分流比为5∶1。结果邻苯二胺、对苯二胺、间苯二胺质量浓度分别在0.996 8~99.680 0μg/m L(r=0.999 5),0.991 4~99.140 0μg/m L(r=0.999 5),1.003 8~100.380 0μg/m L(r=0.999 6)范围内与峰面积线性关系良好,平均回收率分别为89.74%,89.71%,89.20%,RSD分别为1.70%,1.45%,1.68%(n=9);所有样品中均未检出苯二胺。结论该方法可用于药用复合膜中苯二胺的质量控制,苯二胺的限度标准初步确定为不得超过0.05%。
Objective To determine the content of phenylenediamine in laminated films for pharmaceutical packaging and establish the limit standard.Methods The chromatographic column was Shimadzu Rtx-5 capillary column(30 m×0.25 mm,0.25μm),the temperature was 200℃for inlet,220℃for gasification chamber,300℃for flame ionization detector(FID),the flow rate of carrier gas was0.8 m L/min for high purity nitrogen,40 m L/min for hydrogen,400 m L/min for air and 30 m L/min for tail gas.The temperature-programmed was adopted for column temperature(the initial temperature was 100℃,maintained for 1 min,the temperature was raised to200℃at the rate of 20℃/min,maintained for 0 min,and then it was raised to 280℃at the rate of 20℃/min,maintained for 10 min).The split ratio was 5∶1.Results O-Phenylenediamine,p-Phenylenediamine and m-Phenylenediamine showed good linear relationship with peak area in the ranges of 0.9968-99.6800μg/m L(r=0.9995),0.9914-99.1400μg/m L(r=0.9995)and1.0038-100.3800μg/m L(r=0.9996),respectively.The average recoveries were 89.74%,89.71%,89.20%,and the RSDs were1.70%,1.45%and 1.68%(n=9),respectively.No phenylenediamine was detected in all samples.Conclusion The method can be used for quality control of phenylenediamine in laminated films for pharmaceutical packaging and the limit standard of phenylenediamine is not more than 0.05%.
作者
张璞
吴红洋
曹汐
范能全
ZHANG Pu;WU Hongyang;CAO Xi;FAN Nengquan(Chongqing Institue for Food and Drug Conrol,Chongqing,China 401121)
出处
《中国药业》
CAS
2020年第23期43-45,共3页
China Pharmaceuticals
基金
重庆市科研机构绩效激励引导专项[cstc2019jxjl130040]。
关键词
气相色谱法
药用复合膜
苯二胺
含量测定
限度标准
gas chromatography
laminated films for pharmaceutical packaging
phenylenediamine
content determination
limit standard
