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Analytical Methods

Contaminants of Emerging Concern

Pharmaceuticals and Personal Care Products (PPCPs) Methods Development

Other PPCP Links

Since the first reports that Contaminants of Emerging Concern such as pharmaceuticals were occurring in surface waters, a number of questions have been raised regarding their presence in sewage influent, effluent and sludge. At the time of these first reports, no suitable methods were available for sewage influent, effluent and sludge. The Environmental Protection Agency has developed two new state-of-the-art analytical methods to identify and measure certain contaminants of emerging concern, specifically; pharmaceuticals and, steroids and hormones in sewage influent, effluent and sludge.

Number Method Title
1694 Pharmaceuticals and Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS (PDF) (77 pages, 330 K)
1698 Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS (PDF) (69 pages, 290 K)

These methods currently cover over 100 chemicals: 74 pharmaceuticals and personal care products and 27 steroids-hormones; and three wastewater matrices: raw and treated sewage water and sludge.

In addition to the new CEC-related methods developed for this study, EPA has single lab validated a new pesticide method and revised the existing flame retardants (PBDE) method in order to more accurately detect CECs in wastewater samples:

Number Method Title
1614 Brominated Diphenyl Ethers in Water Soil, Sediment and Tissue by HRGC/HRMS (PDF) (87 pp., 417 K)
1699 Pesticides in Water, Soil, Sediment, Biosolids, and Tissue by HRGC/HRMS (PDF) (96 pp., 598 K)

Methods Status

These methods have been peer-reviewed and tested in a single lab. The contaminants in these methods are not currently regulated, nor have the methods been promulgated at 40 CFR Part 136.

Laboratories familiar with environmental analysis should be consulted regarding their ability to perform these methods.

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Contaminants of Emerging Concern in EPA Methods 1694 and 1698

Method 1694: 74 Pharmaceuticals or Personal Care Products in Water, Soil, Sediment, and Biosolids by HPLC/MS/MS
PPCP CAS # Classification
Ibuprofen 15687-27-1 Analgesic
Cimetidine 51481-61-9 Anti-acid reflux
Ranitidine 66357-35-5 Anti-acid reflux
Albuterol 18559-94-9 antiasthmatic
Warfarin 81-81-2 anticoagulant
Carbamazepine 298-46-4 Anticonvulsant
Metformin 657-24-9 anti-diabetic drug
Miconazole 22916-47-8 antifungal agent
Diphenhydramine 58-73-1 Antihistamine
Diltiazem 42399-41-7 antihypertensive
Gemfibrozil 25812-30-0 Antilipemic
Triclocarban 101-20-2 antimicrobial, disinfectant
Triclosan 3380-34-5 antimicrobial, disinfectant
Acetaminophen 103-90-2 Antipyretic, Analgesic
1,7-Dimethylxanthine 611-59-6 Antispasmodic, caffeine metabolite
Digoxin 20830-75-5 cardiac glycoside
Cefotaxime 63527-52-6 Cephalosporin antibiotic
Anhydrochlortetracycline (ACTC) 13803-65-1 chlorotetracycline degradate
Anhydrotetracycline (ATC) 4496-85-9 chlorotetracycline degradate
4-Epianhydrochlortetracycline (EACTC) 158018-53-2 chlorotetracycline degradate
4-Epianhydrotetracycline (EATC) 4465-65-0 chlorotetracycline degradate
4-Epichlortetracycline (ECTC) 14297-93-9 chlorotetracycline degradate
Isochlortetracycline (ICTC) 514-53-4 chlorotetracycline degradate
Sarafloxacin 98105-99-8 Fluoroquinolone antibiotic
Thiabendazole 148-79-8 fungicide and parasiticide
Norgestimate 35189-28-7 Hormonal contraceptives
Digoxigenin 1672-46-4 Immunohistochemical Marker Steroid
Lincomycin 154-21-2 lincosamide antibiotic
Azithromycin 83905-01-5 Macrolide Antibiotic
Clarithromycin 81103-11-9 Macrolide antibiotic
Erythromycin 114-07-8 Macrolide antibiotic
Ormetoprim 6981-18-6 Macrolide antibiotic
Roxithromycin 80214-83-1 Macrolide antibiotic
Tylosin 1401-69-0 Macrolide antibiotic
Virginiamycin 11006-76-1 Macrolide antibiotic
Erythromycin anhydrate 59319-72-1 macrolide antibiotic
Cotinine 486-56-6 nicotine metabolite
Dehydronifedipine 67035-22-7 Nifedipine metabolite
Naproxen 22204-53-1 non-steroidal anti-inflammatory drug
Codeine 76-57-3 opiate
4-Epioxytetracycline (EOTC) 14206-58-7 oxytetracycline degradate
Trimethoprim 738-70-5 Pyrimidine antibiotic
Ciprofloxacin 85721-33-1 Quinoline antibiotic
Clinafloxacin 105956-97-6 Quinoline antibiotic
Enrofloxacin 93106-60-6 Quinolone antibiotic
Flumequine 42835-25-6 Quinolone antibiotic
Lomefloxacin 98079-51-7 Quinoline antibiotic
Norfloxacin 70458-96-7 Quinoline antibiotic
Ofloxacin 82419-36-1 Quinoline antibiotic
Oxolinic acid 14698-29-4 Quinolone antibiotic
Carbadox 6804 07 05 Quinoxaline Antibiotic
Ampicillin 69-53-4 β-lactam antibiotics
Cloxacillin 61-72-3 β-lactam antibiotics
Oxacillin 66-79-5 β-lactam antibiotics
Penicillin V 87-08-1 β-lactam antibiotics
Penicillin G 61-33-6 β-lactam antibiotics
Fluoxetine 54910-89-3 SSRI Antidepressant
Caffeine 58-08-2 Stimulant
Sulfachloropyridazine 80-32-0 Sulfonamide antibiotic
Sulfadiazine 68-35-9 Sulfonamide antibiotic
Sulfadimethoxine 122-11-2 Sulfonamide antibiotic
Sulfamerazine 127-79-7 Sulfonamide antibiotic
Sulfamethazine 57-68-1 Sulfonamide antibiotic
Sulfamethoxazole 723-46-6 Sulfonamide antibiotic
Sulfanilamide 63-74-1 Sulfonamide antibiotic
Sulfathiazole 72-14-0 Sulfonamide antibiotic
Sulfamethizole 144-82-1 Sulfonamide antibiotic
Chlortetracycline (CTC) 57-62-5 Tetracycline antibiotic
Demeclocycline 127-33-3 Tetracycline antibiotic
Doxycycline 564-25-0 Tetracycline antibiotic
Minocycline 10118-91-8 Tetracycline antibiotic
Oxytetracycline (OTC) 79-57-2 Tetracycline antibiotic
Tetracycline (TC) 60-54-8 Tetracycline antibiotic
4-Epitetracycline (ETC) 23313-80-6 Tetracycline degradate

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Method 1698: 27 Steroids and Hormones in Water, Soil, Sediment, and Biosolids by HRGC/HRMS
Steroid/Hormone CAS # Classification
Androstenedione 63-05-8 anabolic agent
Androsterone 53-41-8 hormone metabolite
Equilenin 517-09-9 hormone replacement
Equilin 474-86-2 hormone replacement
17a-Ethynyl Estradiol (EE2) 57-63-6 ovulation inhibitor
Desogestrel 54024-22-5 ovulation inhibitor
Mestranol 72-33-3 ovulation inhibitor
Norethindrone 68-22-4 ovulation inhibitor
Norgestrel 6533-00-2 ovulation inhibitor
Campesterol 474-62-4 Phytosterol (plant sterol)
beta-Sitosterol 83-46-5 Phytosterol (plant sterol)
Stigmasterol 83-48-7 Phytosterol (plant sterol)
Beta-Stigmastanol 83-45-4 Phytosterol (plant sterol)
17a-Estradiol 57-91-0 Sex Hormone
17b-Estradiol (E2) 50-28-2 Sex Hormone
Estriol (E3) 50-27-1 Sex Hormone
Estrone (E1) 53-16-7 Sex Hormone
Progesterone 57-83-0 Sex Hormone
Testosterone 58-22-0 Sex Hormone
17a-Dihydroequilin 651-55-8 Sterol
Cholestanol 80-97-7 Sterol
Cholesterol 57-88-5 Sterol
Desmosterol 313-04-2 Sterol
Ergosterol 57-87-4 Sterol
b-Estradiol-3-benzoate 50-50-0 Sterol
Coprostanol 360-68-9 Sterol
Epi-Coprostanol 516-92-7 Sterol

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