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Purpose of diclofenac sodium is a non-steroidal anti-inflammatory drugs, antipyretic, analgesic and anti-inflammatory effects. Diclofenac sodium mechanism of action is inhibition of cyclooxygenase activity, thereby blocking arachidonic acid into prostaglandins. Meanwhile, it can also promote arachidonic acid in combination with triglyceride (triacylglycerol), to reduce the concentration of intracellular free arachidonic acid, and thus indirectly inhibit leukotriene synthesis. Diclofenac sodium has the role of fast, efficacy, absorption, and a small amount of small, individual differences, side effects and other characteristics, are widely used clinically. Therefore, there is a need to strengthen its monitoring. This article aims to apply two different pre-treatment methods - liquid-liquid extraction (LLE) and solid-phase extraction (SPE), to establish a rapid, sensitive and exclusive in human plasma diclofenac sodium content of GC-MS method. 3, diclofenac sodium control, instruments and materials, Shimadzu gas chromatography - mass spectrometry the instrument (GC/MS-QP2010) TDZ4-WS tabletop centrifuge, DELTA 302 pH meter, of the LG WD700 (MG5055M) Microwave products (China Pharmaceutical and Biological Products Institution are ,100334 -200,302), ibuprofen reference substance (China Pharmaceutical and Biological Products ,100179 -200,302), the 1,3,5 - tribromophenyl (China Pharmaceutical and Biological Products NICPBP) , N, O-bis (trimethylsilyl) trifluoroacetamide (BSTFA) standard solution (Beijing MPS II), heptafluoro butyryl chloride (HFB-Cl) standard solution (manufactured by Tokyo Kasei Kogyo Co., Ltd.) 5. diatomaceous earth (Tokyo Kasei Kogyo Co., Ltd.), blank plasma (blood bank of the First Affiliated Hospital of China Medical University), anhydrous ethanol, ethyl ether, n-hexane, n-butyl propionate, experimental step method: Plasma samples were acidic anti mention, the extract in a microwave heating under silylating processing backward (TMS) Sample GC-MS analysis. Analysis by mass spectrometry in selected ion mode (SIM), the test diclofenac TMS derivatives quantitative selective positive ion detection mass-to-charge ratio of m / z 367, internal standard ibuprofen TMS derivatives quantitative selective positive ion detection quality The charge ratio of m / z 263. Method Two: plasma samples by solid-phase extraction backward sample GC-MS analysis, analysis by mass spectrometry in selected ion monitoring (SIM) mode for the test diclofenac lactam structure quantitative selective positive ion mass to charge ratio m/z214 within standard substance 1,3,5 - tribromophenyl quantitative selective positive ion detection mass-to-charge ratio of m / z 314. LLE and SPE method results using pre-treatment of diclofenac sodium, Diclofenac trimethylsilyl product and diclofenac amide product were obtained, these two goals are volatile product was analyzed, the thermal stability of the compounds in the chromatographic system can achieve a good separation with a suitable internal standard, and therefore suitable for GC-MS analysis. Analysis of the process, the blank plasma treatment of test samples without significant interference. Method, the test retention time of 7.977 min and 12.470 min; the the diclofenac plasma drug concentration of 0.005 to 10 μg of · mL -1 range a good linear relationship (r = 0.9997) minimum The detection limit was 0.5 ng · mL -1 ; recoveries of between 94% to 98%, intra-day RSD were less than 5%. Two internal standard and the test retention time of 6.486 min and 11.761 min; the the diclofenac plasma drug concentration of 0.005 to 10 μg of · mL -1 range a good linear relationship (r = 0.9978), the lowest The detection limit was 0.5ng · mL -1 ; recoveries of between 79% to 88%, intra-day RSD were less than 8%. Conclusion The method is simple, accurate, high-sensitivity, clinical diclofenac sodium plasma concentration can be used for monitoring and forensic toxicology.
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