目的: 建立一种快速、准确测定远红外贴中16个非法添加药物(10种非甾体类抗炎药和6种糖皮质激素药)的方法。方法: 样品经冷凝回流后,用高效液相色谱法(HPLC)及高分辨液质联用法(UPLC-HRMS/MS)对非法添加药物进行定性分析,并使用高效液相色谱法(HPLC)进行含量测定。结果: 16个非法添加药物在相应测定范围内线性关系良好,相关系数均大于0.999;在3个浓度加标水平下,回收率为81.1%~112.7%;RSD为0.010%~2.8%;各药物检测下限为0.05~1.5 μg·mL-1;定量下限为0.2~5 μg·mL-1;35批样品中9批次检出双氯芬酸钠成分,含量为0.56~37.11 mg·贴-1。结论: 该方法操作简便,专属性强,灵敏度、准确度高,适用于远红外贴及同类产品中非法添加药物的检测。
Objective: To establish a rapid and accurate method for the identification and determination of 16 drugs illegally added in far infrared stickers. Methods: Samples were refluxed in methanol. High performance liquid chromatography (HPLC) and liquid chromatography tandem high resolution mass spectrometry (LC-HRMS/MS) were used for qualitative analysis of illegally added drugs, and HPLC was used for content determination. Results: The 16 compounds showed good linear relationship within their ranges, and the correlation coefficients(r) were above 0.999. Under three different concentration levels, the recoveris ranged from 81.1% to 112.7% with the RSDs of 0.010% to 2.8% at the three concentration levels. The LODs were in range of 0.05-1.5 μg·mL-1 and the LOQs were in range of 0.2-5 μg·mL-1. Diclofenac sodium was detected in 9 of the 35 samples in range of 0.56-37.11 mg per sticker. Conclusion: The method is simple, specific, highly sensitive and accurate, and can be used for the detection of the 16 drugs illegally added in far infrared stickers and similar products.
[1] 赖锦坝, 许晓萍, 张龚敏. 远红外贴安全有效性研究[J].中国医疗器械信息, 2019, 25(7): 36
LAI JB, XU XP, ZHANG GM. Far infrared stickers safety and effectiveness study [J].China Med Dev Inf, 2019, 25(7): 36
[2] 毕建云, 战旗, 张震宇. 中药远红外穴位贴的研究进展[J].山东中医杂志, 2020, 39(7): 754
BI JY, ZHAN Q, ZHANG ZY. Research progress on far-infrared acupoint paste with Chinese medicinals [J].Shandong J Tradit Chin Med, 2020, 39(7): 754
[3] 王燕, 王巨才, 王康俊. 远红外痛经理疗贴治疗妇科疾病120例的临床观察[J].中国医疗器械信息, 2019, 25(5): 147
WANG Y, WANG JC, WANG KJ. Clinical observation on 120 cases of gynecological diseases treated by far-infrared dysmenorrheal physical therapy paste [J].China Med Dev Inf, 2019, 25(5): 147
[4] 王琪珊, 王婷玉. 糖皮质激素在类风湿性关节炎中的作用研究进展[J].中国药理学通报, 2018, 34(12): 1647
WANG QS, WANG TY. Research progress of role of glucocorticoids in rheumatoid arthritis [J].Chin Pharmacol Bull, 2018, 34(12): 1647
[5] 张启颖. 糖皮质激素类药物的用药误区及合理用药分析[J].中国医药指南, 2020, 18(25): 45
ZHANG QY. Misunderstanding and rational use of glucocorticoid drugs[J].Guide China Med, 2020, 18(25): 45
[6] 左橙子, 彭文兴. 非甾体抗炎药的安全用药与合理选择[J].中南药学, 2017, 15(5): 639
ZUO CZ, PENG WX. Safety and rational choice of non-steroidal anti-inflammatory drugs[J].Cent South Pharm, 2017, 15(05): 639
[7] 杭桂华. 探讨非甾体类抗炎药不良反应及预防措施[J].大医生, 2019, 4(24): 156
HANG GH. Investigate the adverse reactions and preventive measures of non-steroidal anti-inflammatory drugs [J].Doctor, 2019, 4(24): 156
[8] 汤智慧, 母义明. 关注因药物相互作用导致的医源性库欣综合征[J].药品评价, 2019, 16(3): 7
TANG ZH, MU YM. Focus on iatrogenic Cushing's syndrome caused by drug interactions [J].Drug Eval, 2019, 16(3): 7
[9] 季闽春, 耿晓芳, 殷民德. 非甾体抗炎药物与ACE抑制剂的相互作用[J].中国临床药理学杂志, 2003,19(4): 310
JI MC, GENG XF, YIN MD. Drug interaction between nonsteroid anti-inflammatory drugs and angiotensin converting enzyme inhibitors[J].Chin J Clin Pharmacol, 2003,19(4): 310
[10] 刘治军. 关于药物相互作用几个问题的思考[J].药物不良反应杂志, 2019(6): 401
LIU ZJ. Thoughts on several problems of drug interactions [J].Adv Drug React J, 2019(6): 401
[11] 赵琪,钱叶飞,贾昌平,等. UPLC-DAD快速筛查抗风湿类保健食品及中成药中非法添加的19个化学物质[J].药物分析杂志, 2019, 39(12): 2171
ZHAO Q, QIAN YF, JIA CP, et al. Rapid determination of illegally added chemical drugs in anti-rheumatic Chinese traditional patent medicine and health foods by UPLC-DAD [J].Chin J Pharm Anal, 2019, 39(12): 2171
[12] 孙夏荣,史达,曹玉,等. 超高效液相色谱-串联质谱法同时测定外用贴膏剂中非法添加48个化合物[J].药物分析杂志, 2020, 40(3): 502
SUN XR, SHI D, CAO Y, et al. Simultaneous determination of 48 compounds illegally added in emplastrum by UPLC-MS/MS [J].Chin J Pharm Anal, 2020, 40(3): 502
[13] 凌霄,徐志洲,牛冲.HPLC/MS/MS法检测中药制剂中解热镇痛及糖皮质激素类化学药[J].药物分析杂志,2010,30(7): 1311
LING X, XU ZZ, NIU C. HPLC-MS/MS Detection of relieve pain drugs and glucocorticosteroid in traditional Chinese preparation[J].Chin J Pharm Anal,2010,30(7): 1311
[14] 乜红磊, 张磊. UPLC-MS/MS法检测抗风湿类中药制剂中非法添加的21种糖皮质激素类化学药物[J].中南药学,2020,18(7): 1147
NIE HL, ZHANG L. Detection of 21 illegally added glucocorticoids in anti-rheumatism medicine by UPLC-MS/MS[J].Cent South Pharm, 2020, 18(7): 1147
[15] 何睿偲, 黄艳婷, 雷毅, 等. HPLC法快速筛查抗风湿类中成药或保健食品中21种非法添加化学成分[J].分析测试学报, 2016, 35(11): 1486
HE RS, HUANG YT, LEI Y, et al. Rapid determination of 21 Adulterants in anti-rheumatic Chinese patent drugs of dietary supplements by HPLC[J].J Instrum Anal, 2016, 35(11): 1486
[16] GB/T 16886.12-2017医疗器械生物学评价[S].第12部分:样品制备与参照材料
GB/T-16886.12-2017 Biological Evaluation of Medical Devices[S].Part 12:Sample Preparation and Reference Materials