Leak-tight \folves fil Fittings for Analytical Instrument Applications The leak-tight technology of the SWAGELOK Companies is built into all the products you see here. They work with each other to give you design flexibility You can select sizes, shapes, materials and ratings to handle your service conditions. They're all manufactured to the same standards of precision and quality control. You can count on consistent tolerances, compatible end connections, and reliable seals. They're available locally from Authorized Sales and Service representatives. You can save money through efficient purchasing, controlled inventories, and on-time delivery. SWAGELOK Co. Solon, Ohio 44139 SWAGELOK Canada Ltd., Ontario TUBE FITTINGS
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58 A · ANALYTICAL CHEMISTRY, VOL. 61, NO. 1, JANUARY 1, 1989
These Products are subjects ot paient or patents pending
ANALYTICAL APPROACH spectrum shown in Figure 4a. Higher mass singly charged ions and lower mass fragment ions were observed for authentic succinylcholine. Identical LC/MS/MS experiments performed on the toxic dexamethasone extract pro vided the full-scan product ion mass spectrum shown in Figure 4b. This was identical to the mass spectrum for au thentic succinylcholine (Figure 4a.) We now had conclusive proof that the toxic dexamethasone extract contained suc cinylcholine, which was not present in the control dexamethasone extract. Furthermore, it was determined by LC/MS quantitative analysis studies that the concentration of succinylcho line in the injectable dexamethasone was 8.8 mg/mL. A 15-kg dog treated with 5 mL of this solution would have received 44 mg or 2.93 mg/kg of succi nylcholine. The standard dosage of this drug is 0.3 mg/kg. It is little wonder that the animals succumbed to the ac cidental treatment of succinylcholine described here. Postdiscovery analyses
After the toxic analyte was identified, a renewed effort was made to detect suc cinylcholine by conventional methods. TLC was performed on silica gel plates using the original drug solutions rather than the extracts. The best solvent sys tem found was a 1:1 solution of chloro form and methanol. This removed the polyethylene glycols and parabens from the analyte of interest, which re mained at the origin of the TLC plate. Spraying the plate with Dragendorf s reagent yielded a bright red color that turned black after overspraying with copper chloride and sodium nitrate. This was consistent with the authentic standard. Preparative TLC for capillary GC/ MS analysis consisted of scrapes from the origin (R/ = 0.0) after development in the 1:1 chloroform/methanol solu tion. The scrapes were eluted from the silica gel using acidified water, diluted with methanol, and concentrated to dryness under nitrogen in a hot water bath. The residue was redissolved in methanol and chloroform (1:4) and an alyzed by capillary GC/MS. An injection port pyrolysis technique previously reported (6) was used to ver ify the presence of succinylcholine by standard GC/MS. Instrumentation consisted of a Hewlett-Packard Model 5890 capillary gas chromatograph cou pled to a Model 5970 mass selective detector. The column employed was an HP 100% methylsilicone fused-silica capillary column (0.2 mm i.d. X 12 m). The initial oven temperature (170 °C) was held for 1 min and was followed by
