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Volume 40 Issue 3
Jul.  2022
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LU Songwei, LUO Jinqian, YU Huihua, CHEN Fangjian. Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2022, 40(3): 274-276. doi: 10.12206/j.issn.1006-0111.202102016
Citation: LU Songwei, LUO Jinqian, YU Huihua, CHEN Fangjian. Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2022, 40(3): 274-276. doi: 10.12206/j.issn.1006-0111.202102016

Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC

doi: 10.12206/j.issn.1006-0111.202102016
  • Received Date: 2021-02-22
  • Rev Recd Date: 2022-01-10
  • Available Online: 2023-11-06
  • Publish Date: 2022-05-25
  •   Objective  To establish the HPLC method of assay for diphenhydramine hydrochloride in compound diphenhydramine cream.   Method   HPLC analysis was carried on ACE5C18S/N-A66766 column (150 mm×4.6 mm, 5 µm) with the mobile phase of methanol-water-triethylamine (70:30:0.67, adjusting pH to 6.50 with phosphoric acid) at room temperature. The detection wavelength was set at 230 nm and the flow rate was 1.0 ml/min. The analyte was extracted from the cream and 20 μl of sample was injected.   Results  The calibration curve of diphenhydramine hydrochloride was linear in the range of 39.52-197.6 µg/ml (r=0.999 7). The average recovery of diphenhydramine hydrochloride was 100.5% (RSD=1.25%, n=9). The repeatability of the method was expressed using RSD with 0.78% (n=6). The results of assay were 101.3%, 99.83% and 99.62%.   Conclusion   The method is accurate, sensitive, selective and repeatable, which can be applied for improving the quality standard of compound diphenhydramine cream.
  • [1] 李云霞, 周娜, 王波云, 等. 高效液相色谱法测定硼黄栓中盐酸苯海拉明和呋喃唑酮的含量[J]. 解放军医药杂志, 2019, 31(7):100-104. doi:  10.3969/j.issn.2095-140X.2019.07.024
    [2] 刘珊, 蒋琳兰, 谢新民, 等. HPLC法同时测定氯苯醇溶液中氯霉素和盐酸苯海拉明的含量[J]. 中国药房, 2016, 27(27):3847-3849. doi:  10.6039/j.issn.1001-0408.2016.27.34
    [3] 韩凌, 王新霞, 吕磊, 等. HPLC法同时测定多效防护霜中盐酸苯海拉明、甲氧基肉桂酸辛酯和水杨酸辛酯的含量[J]. 药学实践杂志, 2019, 37(6):508-511. doi:  10.3969/j.issn.1006-0111.2019.06.007
    [4] 杨涛, 靳婷, 王荣, 等. 建立快速检测制剂中盐酸苯海拉明含量的方法[J]. 解放军医药杂志, 2017, 29(6):110-112.
    [5] 廖娴, 黄月纯, 丘振文, 等. HPLC法测定苯海拉明麻黄素滴鼻液中盐酸苯海拉明含量[J]. 亚太传统医药, 2018, 14(5):33-35.
    [6] 白林, 范金钊, 蔡乐, 等. HPLC法测定盐酸苯海拉明乳膏的含量[J]. 中国药物应用与监测, 2014, 11(6):348-350.
    [7] SABINS D, DIEP T, MCCARTAN P, et al. Stability and compatibility of diphenhydramine hydrochloride in intravenous admixtures: a new look at an old drug[J]. Hosp Pharm,2019,54(5):330-334. doi:  10.1177/0018578718802586
    [8] 国家药典委员会. 中华人民共和国药典(2020年版)二部[S]. 北京: 中国医药科技出版社, 2020: 1199.
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Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC

doi: 10.12206/j.issn.1006-0111.202102016

Abstract:   Objective  To establish the HPLC method of assay for diphenhydramine hydrochloride in compound diphenhydramine cream.   Method   HPLC analysis was carried on ACE5C18S/N-A66766 column (150 mm×4.6 mm, 5 µm) with the mobile phase of methanol-water-triethylamine (70:30:0.67, adjusting pH to 6.50 with phosphoric acid) at room temperature. The detection wavelength was set at 230 nm and the flow rate was 1.0 ml/min. The analyte was extracted from the cream and 20 μl of sample was injected.   Results  The calibration curve of diphenhydramine hydrochloride was linear in the range of 39.52-197.6 µg/ml (r=0.999 7). The average recovery of diphenhydramine hydrochloride was 100.5% (RSD=1.25%, n=9). The repeatability of the method was expressed using RSD with 0.78% (n=6). The results of assay were 101.3%, 99.83% and 99.62%.   Conclusion   The method is accurate, sensitive, selective and repeatable, which can be applied for improving the quality standard of compound diphenhydramine cream.

LU Songwei, LUO Jinqian, YU Huihua, CHEN Fangjian. Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2022, 40(3): 274-276. doi: 10.12206/j.issn.1006-0111.202102016
Citation: LU Songwei, LUO Jinqian, YU Huihua, CHEN Fangjian. Diphenhydramine hydrochloride asaay in compound diphenhydramine cream by HPLC[J]. Journal of Pharmaceutical Practice and Service, 2022, 40(3): 274-276. doi: 10.12206/j.issn.1006-0111.202102016
  • 复方苯海拉明乳膏是由盐酸苯海拉明、醋酸地塞米松、樟脑、薄荷脑等制成,是长海医院院内特色制剂,临床使用多年,主治过敏性皮炎、接触性皮炎及皮肤瘙痒症等皮肤病,疗效显著。原质量标准仅测定醋酸地塞米松含量,对反映药效的盐酸苯海拉明未建立质控方法。本研究建立测定复方苯海拉明乳膏中盐酸苯海拉明含量的HPLC法,为提高复方苯海拉明乳膏的质量控制标准提供参考。

    • 岛津高效液相色谱仪(包括LC-20AD泵、SPD-M20A二极管阵列检测器、CBM-20A控制器和LC solution工作站,日本岛津公司),XS205DU 电子天平(瑞士梅特勒-托利多仪器有限公司),DL- 720A 超声波清洗器(上海之信仪器有限公司)等。

    • 复方苯海拉明乳膏(规格:20 g:盐酸苯海拉明200 mg与醋酸地塞米松10 mg,长海医院药学部自制,批号:201008、201104、201105);盐酸苯海拉明对照品(含量99.2%,启东东岳药业有限公司,批号:DH-201909101);甲醇为色谱纯,无水乙醇、磷酸均为分析纯,水为蒸馏水。

    • 色谱柱为ACE5C18S/N-A66766柱(150 mm×4.6 mm,5 µm,英国ACE公司);流动相为甲醇-水-三乙胺(70∶30∶0.67,用磷酸调pH为6.5);流速为1.0 ml/min;柱温为室温;检测波长为230 nm;进样量为20 µl。

    • 精密称取盐酸苯海拉明对照品1.976 g,置100 ml量瓶中,加甲醇适量使溶解并稀释至刻度,摇匀,即得浓度为1.976 mg/ml的盐酸苯海拉明对照品储备液。

    • 精密称取本品1 g(约相当于盐酸苯海拉明10 mg),置烧杯中,加甲醇约25 ml,置水浴上加热,搅拌,使其溶解,再置冰浴中冷却,滤过,滤液置100 ml量瓶中,同法提取3次,滤液并入量瓶中,用甲醇稀释至刻度,摇匀,得供试品溶液。

    • 按本品处方制备不含盐酸苯海拉明的空白乳膏,再按供试品溶液制备方法制备成阴性对照溶液。

    • 按照“2.1”项下色谱条件,分别精密吸取对照品溶液、供试品溶液和阴性对照溶液各20 µl进样测定。结果表明,供试品溶液色谱图中,在与对照品溶液色谱图相同的保留时间上有相同的色谱峰,出峰时间为7.8 min, 理论塔板数按盐酸苯海拉明峰计算大于8 000,与相邻峰的分离度大于2.0;而阴性对照品在此处则无色谱峰,说明乳膏基质及其他成分在此色谱条件下对盐酸苯海拉明测定无干扰,表明方法专属性良好,结果见图1

    • 精密量取“2.2.1”项下盐酸苯海拉明对照品储备液1.0、2.0、3.0、4.0、5.0 ml分别置50 ml量瓶中,加甲醇稀释至刻度,摇匀,得到系列浓度为39.52、79.04、118.6、158.1、197.6 µg/ml的盐酸苯海拉明对照品溶液。精密吸取对照品系列溶液各20 µl,按照“2.1”项下色谱条件进样,测定峰面积。以峰面积(A)为纵坐标,浓度(C)为横坐标,绘制标准曲线,得到回归方程:A=16 944C+14 047,r=0.999 7。结果表明,盐酸苯海拉明在39.52~197.6 µg/ml范围内线性关系良好。

    • 精密吸取“2.4”项下浓度为79.04 µg/ml的对照品溶液20 µl,按照“2.1”项下色谱条件连续进样6次,按峰面积计算盐酸苯海拉明的日内精密度为0.82%(n=6)。

    • 精密吸取“2.4”项下浓度为79.04 µg/ml的对照品溶液20 µl,按照“2.1”项下色谱条件每日测定1次,连续测定5 d,记录峰面积,计算日间精密度为1.08%(n=5)。表明仪器精密度良好。

    • 取同一批号(201008)样品,按“2.2.2”项下方法制备6份供试品溶液,按含量测定方法测定,代入回归方程计算含量,计算得到盐酸苯海拉明的含量为100.2%,RSD为0.78%(n=6),表明方法的重复性良好。

    • 按“2.2.2”项下方法制备供试品溶液,分别在0、2、4、6、8 h各进样1次,记录峰面积,计算得到盐酸苯海拉明的RSD为0.59%(n=5),表明供试品溶液在8 h内稳定。

    • 精密称定9份不含盐酸苯海拉明的空白乳膏各1.0 g,置烧杯中,分别加入已知浓度的盐酸苯海拉明对照品适量,加甲醇约25 ml,置水浴上加热,搅拌,使其溶解,再置冰浴中冷却,滤过,滤液置100 ml量瓶中,同法提取3次,滤液并入量瓶中,用甲醇稀释至刻度,摇匀,得相当于标示量的80%、100%、120%的模拟样品各3份,按含量测定方法测定,代入回归方程计算含量,并计算样品的回收率。结果为盐酸苯海拉明的平均回收率100.5%(RSD=0.26%,n=9),见表1

      加入量(m/mg)测得量(m/mg)回收率(%)平均回收率(%)
      7.90 7.92±0.09100.25±1.08100.47
      9.88 9.92±1.16100.40±1.17
      11.8611.95±0.19100.76±1.59
    • 取3个批号的复方苯海拉明乳膏,按“2.2.2”项下方法制备供试品溶液,按照“2.1”项下色谱条件分别进样测定,记录峰面积,计算盐酸苯海拉明的含量分别为标示量的101.3%、99.83%和99.62%,结果见表2

      批号含量(mg/g)RSD(%)
      20100810.13±0.111.12
      201104 9.98±0.150.57
      201105 9.96±0.220.66
    • 盐酸苯海拉明测定的关键在于样品中盐酸苯海拉明的提取,盐酸苯海拉明在水中极易溶解,在乙醇或三氯甲烷中易溶,熔点为167~171℃。本实验比较了不同溶剂如水、乙醇、甲醇及其混合液对样品溶解效果的影响,结果显示,用水为溶剂时,样品不溶,而采用甲醇作为溶剂提取回收率高,且样品溶液进入色谱系统不会有不溶物质析出。供试品为水包油型乳膏,其基质在常温下并不能充分溶解,本研究采用甲醇水浴加热至80℃左右,使供试品中的基质和盐酸苯海拉明完全溶解,再通过冰浴冷却除去乳膏剂中的基质,减少对盐酸苯海拉明的干扰和色谱柱的污染,从而获得相对理想的结果。

    • 本研究参考相关文献[1-2],将对照品溶液和供试品溶液在200~400 nm进行扫描,结果发现,盐酸苯海拉明对照品在258 nm波长处有最大吸收,但供试品在258 nm波长处受杂质峰的影响较大,而230 nm波长处盐酸苯海拉明不受杂质、辅料和溶剂的干扰,因此选择230 nm作为其检测波长。

    • 本研究在测定盐酸苯海拉明时,经文献检索[3-7]和《中华人民共和国药典》[8]的收载,对文献和药典中提到的各种流动相分别进行了考察,结果显示,选用甲醇-水(70:30)作为流动相时,分离度较好,且出峰时间适中,但苯海拉明为碱性药物,色谱峰拖尾严重,加入三乙胺,可有效改善色谱峰峰型。

    • 本实验旨在对原有质量标准进行提升,原质量标准中已有醋酸地塞米松含量的测定方法,故本实验仅考察盐酸苯海拉明的含量测定方法。

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