Study Of The Illegal Additives Detection Method In The Cold Medicine Of Traditional Chinese Medicine

Objective: To ensure clinical medication safety. Do some detection method researchon cold medicine of traditional Chinese medicine. To establish a comprehensive detectionmethod, including TLC(Thin-Layer Chromatography)、UPLC (High Performance Liquid)and UPLC-MS, to identify illegal additives in the cold medicine of traditional Chinesemedicine and some related preparations accurately and fast. To guarantee the clinicalmedication safety of the people and provide technical support for supervision overpharmaceutical.Method: According to the clinical manifestations of the common cold，confirm possiblyillegally added chemicals; Preliminary screening seven kinds of illegally added chemicalcomposition in cold resistance medicine by the thin-layer chromatography; Gradient elutionwas used with the mobile phase consisted of water and methanol at1mL·min–1,Simultaneous determination illegal additives of moroxydine hydrochloride、acetaminophen、caffeine、aminopyrine and phenacetin by high-performance liquid chromatography in thecold medicine of traditional Chinese medicine; Ultra performance liquid chromatographytandem three quadrupole mass spectrometer was adopted, the mobile phase consisted ofammonium acetate and methanol at a flow rate0.2mL·min-1. equipped electrosprayionization (ESI)，and multiple reaction monitoring, The relative intensities of the detectedqualitative ion pairs using for qualitative，integrating the signals of the detected quantitativeion pairs using for quantitative;Simultaneous determination illegal additives ofacetaminophen、caffeine、chlorphenamine maleate、pseudoephedrine hydrochloride、diclofenac sodium、aminopyrine、moroxydine hydrochloride and prednisone aectate byUPLC-MS in the cold medicine of traditional Chinese medicineResults:1、 Screening for seven kinds of thin layer chromatography conditions,Eventually confirmed the terms of the following three thin layer chromatography to identifypseudoephedrine hydrochloride、phenacetin、aminopyrine、acetaminophen、diclofenac sodium、caffeine、prednisone aectate：The identify of pseudoephedrine hydrochloride：with trichloromethane-methanol-StrongAmmonia Solution (20:5:0.5) as developer and ninhydrin water as coloration using silica gelG.The identify of phenacetin、aminopyrine、acetaminophen and diclofenac sodium：with ethylacetate-dichloromethane-glacial acetic acid Solution (20:5:0.5) as developer using silicagel GF254. Examined under Uv lamp at254nmThe identify of caffeine and prednisone aectate：with dichloromethane-aether-methanol-water Solution (20:5:0.5) as developer using silica gel GF254,examined under Uv lamp at254nm2、 Simultaneous determination illegal additives of moroxydine hydrochloride、acetaminophen、 caffeine、 aminopyrine and phenacetin by high-performance liquidchromatography in the cold medicine of traditional Chinese medicine; they have a goodlinear correlation of was observed repectively within the range of0.2136～1.602mg·L-1、0.2176～2.176mg·L-1、0.2012～2.102mg·L-1、0.4008～2.004mg·L-1、0.204～2.04mg·L-1;linear equation respectively are Y＝5.7948X+1.1514， r=0.9999，average recovery is95.79%，RSD is2.10%；Y＝8.464X-0.1752， r=0.9999，average recovery is95.74%，RSD is0.64%；Y＝1.5347X+0.7281， r=0.9996，average recovery is97.60%，RSD is1.49%；Y＝3.6718X+0.2587， r=0.9999，average recovery is98.92%，RSD is0.86%；Y＝7.5854X+0.4811， r=0.9999，average recovery is97.70%，RSD is0.95%3、Simultaneous determination illegal additives of acetaminophen、caffeine、chlorphenaminemaleate、pseudoephedrine hydrochloride、diclofenac sodium、aminopyrine、moroxydinehydrochloride and prednisone aectate by UPLC-MS in the cold medicine of traditionalChinese medicine；equipped multiple reaction monitoring，The relative intensities of thedetected qualitative ion pairs using for qualitative，integrating the signals of the detectedquantitative ion pairs using for quantitative．they have a good linear correlation of wasobserved repectively within the range of2.176～27.10μg·L-1、1.006～20.12μg·L-1、0.497～9.94μg·L-1、1.035～25.875μg·L-1、0.4915～9.83μg·L-1、0.510～8.16μg·L-1、2.136～10.6μg·L-1、0.492～9.84μg·L-1，linear equation respectively are Y=36997X+87979，r=0.9991，average recovery is92.43%，RSD is2.44%；Y=60857X+99131，r=0.9997，average recovery is97.75%，RSD is1.69%；Y=355134X+9955.1，r=0.9998，average recovery is89.77%，RSD is5.14%；Y=317534X+619766，r=0.9997，average recovery is87.87%，RSD is4.57%；Y=5204.4X-31.960，r=0.9997，average recovery is88.17%，RSD is5.03%；Y=15911X+5992.5，r=0.9994，average recovery is87.70%，RSD is4.56%；Y=7429.6X+30941，r=0.9995，average recovery is89.31%，RSD is4.84%；Y=7472.2X+1195.6，r=0.9998，average recovery is90.67%，RSD is2.84%。Conclusion: The three methods of TLC(Thin-Layer Chromatography) are simple、rapid and specific，can be used to identify seven drugs illegally added for primary sector; themethod of HPLC is stable and reliable, can be used to identify five drμgs illegally added forprecisely quantization; the method of UPLC-MS is specific and sensitive, can be used toidentify the illegally adulterated in traditional Chinese medicines of the anti-cold drugsqualitative and quantitative.