Instrumentation: clean sampling car
Apparatus: sampler (solid: probe, stainless steel spoon, tweezers, tongs; liquid: medicinal pipettes, beakers, spoons, viscous liquids with glass rods), sample containers (beakers. wide-mouth bottles, stoppered conical bottles, plastic bags, self-sealing bags), auxiliary tools (gloves, scissors, paper, pens, stickers, alcohol cotton wool), Wide-mouth flasks, stoppered conical flasks, plastic bags, self-sealing bags), auxiliary tools (gloves, scissors, paper, pens, self-adhesive labels, alcohol swabs, etc.)
Two, process water sampling SOP
Sampling tools: clean stoppered conical flasks (sanitation and hygiene inspection sampling sterilized stoppered conical flasks, sterilized alcohol cotton balls)
Three, the titrant and the standard liquid preparation SOP
Instruments and appliances: one hundred thousand electronic analytical balance, constant temperature drying oven, buret, pipette, volumetric flasks
1, sulfuric acid titrant [analytical purity of sulfuric acid, the benchmark anhydrous sodium carbonate, methyl red-bromo-cresol green indicator]
2, hydrochloric acid titrant [analytical purity of hydrochloric acid, the benchmark anhydrous sodium carbonate, methyl red-bromo-cresol green, onyx mortar and bowl, with a lid of the magnetic crucible]
3, hydrogen titrant and standard solution preparation SOP
. p>3, sodium hydroxide titrant [analytically pure sodium hydroxide, benchmark potassium hydrogen phthalate, phenolphthalein indicator solution, polyethylene plastic bottles (stopper with 2 holes, holes inserted into a glass tube, 1 tube connected to the soda-lime tube, 1 tube for the use of suction out of the liquid), agate mortar, weighing flask]
4, silver nitrate titrant [silver nitrate, the benchmark sodium chloride, calcium carbonate, dextrin, fluorescent yellow Indicator solution, brown glass bottle with glass stopper]
5, sodium thiosulfate titrant [analytically pure sodium thiosulfate, anhydrous sodium carbonate, the benchmark potassium dichromate, potassium iodide, starch indicator solution, iodine bottles]
6, disodium ethylenediamine tetraacetic acid titrant [disodium ethylenediamine tetraacetic acid, the benchmark zinc oxide, ethanol 0.025% of methyl red, ammonia test solution, ammonia - ammonium chloride buffer ( PH10.0), chromium black T, glass stoppered bottle]
7, potassium permanganate titrant [analytically pure potassium permanganate, benchmark sodium oxalate, sulfuric acid, pendant glass filter, glass stoppered brown glass vials]
8, iodine titrant [analytically pure iodine, benchmark arsenic trioxide, potassium iodide, hydrochloric acid, sodium hydroxide titrant (1mol/L), sulfuric acid titrant (0.5mol/L ), sodium bicarbonate, methyl orange indicator solution, starch indicator solution, pendant glass filters, brown fine-mouthed vials, brown glass stoppered glass vials]
9, perchloric acid titrant [anhydrous glacial acetic acid, acetic anhydride, perchloric acid (70% to 72%), the benchmark of potassium hydrogen phthalate, crystalline violet indicator solution, brown glass vials]
Division, microbiological examination of the SOP
Instruments and Equipment: constant temperature incubator, biochemical incubator, constant temperature water bath, refrigerator, ultra-clean bench, biological microscope, magnifying glass, electric constant temperature drying oven, electric pressure sterilizer, drug balance.
Apparatus: flat dish, pipette (1ml, 10ml), scissors or tweezers (sterilized),
Reagents:
1, Diluent (0.9% sterile sodium chloride solution)
2, Control bacterial solution [take 1 platinum ear of fresh culture from the slant of nutrient agar medium of Escherichia coli [CMCC(B)44 102], inoculate it into nutrient broth medium], 40% potassium hydroxide test solution [take 40g of potassium hydroxide, add water and dissolve into 100ml].
3, 6% α-naphthol ethanol test solution: take 6.0g of α-naphthol, add anhydrous ethanol and dissolve it into 100ml.
4, indigo matrix test solution [p-dimethylaminobenzaldehyde, pentanol (or butanol, concentrated hydrochloric acid, or p-dimethylaminobenzaldehyde, 95% ethanol)
5, methyl red indicator solution [methyl red, 95% ethanol], bromo-muskweedol blue indicator solution [bromo-muskweedol blue indicator solution]. liquid [bromo muscovado phenol blue, 1 mol / L sodium hydroxide solution]
6, acidic magenta indicator (color change range PH6.0 ~ 7.4, yellow → red) [acidic magenta, 1 mol / L sodium hydroxide solution]
7, has been sterilized medium [bacterial counting nutrient agar: molds, yeasts, counting with rosmarinic acid sodium agar, liquid preparations containing honey, syrup, add another YPD agar].
8, E. coli examination [bile salt lactose medium, uninoculated MUG medium, indigo matrix test solution, eosin methylene blue agar plate or MacConkey agar plate], abnormal for indigo matrix test, methyl red test, acetyl methyl alcohol generation test, citrate utilization test and Gram staining, microscopic examination
9, medium preparation method: medium sterilization conditions 121 ℃ 20 minutes. Adjust PH to weak alkaline, 7.2±0.2 after sterilization
1) Nutritional broth medium [peptones 10g, sodium chloride 5g, 1000ml meat infusion], nutritional agar medium [according to the former method, add 15-20g agar]
2) sodium rose red agar medium [peptones 5g, sodium rose red 0.0133g, glucose 10g, magnesium sulfate 0.5g agar 15-20g, potassium dihydrogen phosphate 1g, water 1000ml]
(3) Yeast leaching powder peptones glucose agar medium (YPD) [peptones 10g, agar 15-20g, dextrose 20g, yeast leaching powder 5g, water 1000ml]
(4) Bile Salt Lactose Medium (BL) [ Potassium dihydrogen phosphate 1.3g, Lactose 5g, peptones 10g 5g of sodium chloride, bovine bile salt (or sodium deoxycholate 0.5g) 2g, dipotassium phosphate 4.0g, water 1000ml]
(5) Eosin Methylene Blue Agar Medium (EMB) [Nutrient Agar Medium Theory 100ml, Eosin Sodium Indicator Solution 2ml, 20% lactose solution 5ml, Methylene Blue Indicator Solution 1.3~1.6ml]
(6) MacConkey Agar medium (MacC) [peptones 20g, 1% neutral red indicator solution 3ml, lactose 10g, sodium chloride 5g, agar 15-20g, bovine bile salts 5g, water 1000ml]
(7) 4-methylumbelliferyl glucosinolate (MUG) medium [peptones 10g, potassium dihydrogen phosphate 0.9g, ammonium sulphate 5g, disodium hydrogen phosphate (anhydrous) 6.2g, manganese sulphate 0.5mg, sodium sulfite 40mg, zinc sulfate 0.5mg, sodium sulfite 40mg, magnesium sulfate 0.1g, MUG75mg, sodium chloride 10g, water 1000ml, calcium chloride 50mg]
(8) Peptone water medium [Tryptone 10g, water 1000ml, sodium chloride 5g]
(9) Phosphate Glucose Peptone Water Medium [ Peptone 7g, dipotassium hydrogen phosphate 3.8g, glucose 5g, water 1000ml]
(10) citrate medium [sodium chloride 5g, sodium citrate (anhydrous) 2g, magnesium sulfate 0.2g, bromine musk oxalate phenol blue indicator solution 20ml, dipotassium hydrogen phosphate 1.0g, agar 15-20g, ammonium dihydrogen phosphate 1g, water 1000ml]
Note: the used Note: The agar used should be free of free sugar, soaked and rinsed with water before use.
V. Cleanliness test SOP
Dust particles (laser dust particle counter, sampling tube), settled bacteria [autoclave, constant temperature incubator, magnifying glass, Petri dishes (generally take Φ90mm × 15mm borosilicate glass Petri dishes), ordinary broth agar medium], illuminance meter.
VI. Coliform examination SOP
Instruments and equipments used: microscope, Gram staining equipment, constant temperature incubator, refrigerator, magnifying glass, general laboratory instruments
Lactose peptone culture solution (peptone 10g, beef paste 3g, lactose 5g, sodium chloride 5g, bromo-cresol violet ethanol liquid 1ml, water 1000ml
Duchenne tubes with test tubes, autoclave sterilizer), triple concentration of lactose peptone culture solution, erythromelan medium
seven, thin-layer chromatography procedures
Instrumentation and apparatus: glass plate (10cm × 10cm, 10cm × 15cm, 20cm × 10cm, 20cm × 20cm, 5cm × 20cm), drying oven, sampling device (flat head) Micro-sampler, capillary), unfolding room (flat-bottomed or double-slot chromatography cylinder), mortar, glass rod, thin-layer plate spreader, oven
Adsorbent or carrier: the most commonly used silica gel G, silica gel GF254, silica gel H, silica gel HF254, with water or 0.2-0.5% sodium carboxymethylcellulose aqueous solution in the right amount to make a homogeneous paste
Eight, high-performance liquid chromatography operating procedures
High purity reagents formulated mobile phase, if necessary, according to the ultraviolet spectrophotometry solvent check, should meet the requirements; water should be freshly prepared high-purity water, can be produced with super-pure water purifier or with redistilled water. Where the pH value of the mobile phase, the use of precision pH meter should be adjusted. The prepared mobile phase should be filtered through a suitable 0.45um membrane and degassed before use. Should be prepared in sufficient quantities of mobile phase in time to be used
nine, melting point method operating procedures
Instruments and appliances: heating container, stirrer, thermometer (with a 0.5 ℃ scale, the height of the sub-dip line should be between 5Omm to 8Omm), capillary tube (inner diameter of 0.9 ~ 1.1 lmm), mortar and pestle, flat flasks
Temperature transfer liquid: water (80 ℃) Below), silicone oil or liquid paraffin (above 80 ℃)
Melting point standard: supplied by the China National Institute for the Control of Pharmaceutical and Biological Products, phosphorus pentoxide desiccator stored away from light
Ten, the relative density method operating procedures
Instrumentation: Specific Gravity Bottle, Weiss Specific Gravity Scale, specific gravity, balances, thermostatic baths, 100 ml measuring cylinders
Xi Minimum loading check method operating procedures
Instruments and utensils: balance, syringe (5, 10, 20 and 50m1), measuring cylinder (100, 200 and 500m1)
XII, pH determination method operating procedures
Standard buffer used for instrumental calibration:
1, acid potassium trihydrogen standard buffer (pH1.68 25 ℃): precision weighing in the water at the same time, the standard buffer is used for the determination of pH value. )
1, acid trihydrogen potassium buffer (pH1.68 25 ℃): precision weighing in 54 ℃ ± 3 ℃ dry 4 ~ 5 hours of potassium oxalate [KH3 (C2O4) 2?2H2O] 12.61g, add water to make the dissolution and weighing release to 1000ml.
2, benzene dicarboxylic acid potassium hydrogen standard buffer (pH4.00 25 ℃): precision weighing in 115 ℃ ± 5 ℃ drying for 2 ~ 3 hours of potassium hydrogen phthalate [ KHC8H4O4] 10.12g, add water to dissolve and dilute to 1000ml.
3, acid salt standard buffer (pH6.86 25 ℃): precision weighing in 115 ± 5 ℃ dry for 2 ~ 3 hours of anhydrous disodium hydrogen phosphate 3.533g and potassium dihydrogen phosphate 3.387g, add water to dissolve and dilute to 1000ml.
4, Acid salt standard buffer (pH7.41 25 ℃): precision weighing in 115 ± 5 ℃ dry 2 ~ 3 hours of anhydrous disodium phosphate 4.303g and potassium dihydrogen phosphate 1.179g, add water to dissolve and dilute to 1000ml.
5, sand standard buffer (pH9.18 25 ℃): precision weighing of borax (Na2B4O7?10H2O) 3.80g (pay attention to avoid weathering), add water to dissolve and dilute to 1000ml, placed in a polyethylene plastic bottle, tightly corked, avoid contact with carbon dioxide in the air.
Thirteen, moisture determination method operating procedures
Drying method: analytical balance, flat weighing flasks, electric constant temperature drying oven.
Toluene method: toluene, analytical balance, electric heating jacket or water bath, short-necked round-bottomed flasks, moisture determination tubes, straight condensing tubes, electric constant temperature drying oven, glass beads
Decompression drying method: Petri dishes, decompression drier, weighing flasks, anhydrous calcium chloride desiccant tubes, fresh phosphorus pentoxide desiccant, decompression desiccant (in a decompression desiccant with a diameter of 30cm).
Fourteenth, the loading difference and weight difference checking method operating procedures
Instruments and utensils: analytical balance (sensitivity 1mg or 0.1mg), flat weighing flasks, flat-tipped surgical forceps, gloves, measuring cylinders, beakers
Fifteenth, organochlorine pesticide residue determination method operating procedures
Instrument: gas chromatography
Control reserves Liquid preparation: hexachlorohexane (BHC), DDT (DDT) and pentachloronitrobenzene (PCNB) pesticide control, petroleum ether
Medicinal material test preparation: 100 ml stoppered conical flasks, acetone, ultrasonic, sodium chloride, methylene chloride, anhydrous sodium sulfate, water bath concentration, 10 ml stoppered centrifugal tubes, sulfuric acid, centrifugal machine (3,000 rpm), a scale Concentration bottle, rotary evaporator 40 ℃ (or with nitrogen) concentration
16, ash determination method operating procedures
Instruments and utensils: pulverizer, Pharmacopoeia sieve (No. 2), analytical balance, crucibles, electric furnaces, high-temperature resistance furnace, electric constant temperature drying oven, desiccators, water baths, funnels, ashless filter paper, pipettes, beakers, pipettes, volumetric flasks, bottles of reagents, crucible clamp.
Reagents and preparation: dilute hydrochloric acid solution (measure hydrochloric acid 234 ml, dilute with water to 1000 ml), 10% ammonium nitrate solution (weighing ammonium nitrate 10 g, dilute with water to 100 ml)
XVII, incandescent residue checking method of operation
Instruments and appliances: one ten thousandth of the analytical balance, high temperature furnace, crucible, crucible, fume hood.
The test drug and test solution: sulfuric acid (analytical purity)
Eighteen, leachate determination method operating procedures
Instrumentation and equipment: pulverizer, analytical balance, Pharmacopoeia sieve (No. 2), stoppered conical flasks, pipettes, evaporation dishes, water baths, desiccators, electrothermal constant-temperature drying oven, condensate tube.
Reagents: purified water, methanol, ethanol.
Nineteen, hand sterilization situation check SOP
Instruments and reagents: nutrient agar, Petri dishes, thermostat
Twentieth, the General Rules for the Determination of Medicinal Herbs
Fluorescence identification method (ultraviolet light lamps), the micro-sublimation method (asbestos plate with a circular hole of about 2 cm in diameter, a metal circle of 8 mm, slides, alcohol lamps, microscope)